CN103627944A - Powder metallurgy rare earth super-magnetostrictive bar material and preparation technology therefor - Google Patents

Abstract

The invention discloses a powder metallurgy rare earth super-magnetostrictive bar material and a preparation technology therefor in the technical field of rare earth functional materials. A material assembly matching method is employed that elementary substance powders of two rare earth materials of lanthanum (La) and cerium (Ce) with large scale are directly doped in elementary substance powders of three ferromagnetic metal materials of iron (Fe), nickel (Ni) and cobalt (Co). A plurality of powder metallurgy innovative technologies of ultrasonic solid-phase homogeneous mixing, isostatic pressing compression molding polarization, continuous and gradual sintering fixing and the like are employed for processing and manufacturing of the bar material. In the preparation, typical material characteristics of rare earth materials such as growth chain crystal grain molecule structure and sagging and creeping resistances are fully used, after the rare earth materials with a large proportion and the ferromagnetic metal materials are subjected to assembly and chemical combination, strong dispersion strengthening effect and embedding effect can be displayed, thus the processed powder metallurgy rare earth super-magnetostrictive bar material product has high magnetostrictive strain coefficients and good mechanical and physical properties, and the application range of the bar material product is extended greatly.

Description

Powder smelting rareearth super magnetostrictive bar and technology of preparing thereof

Technical field

The present invention relates to Rare Earth Functional Materials, relate to specifically a kind of powder smelting rareearth super magnetostrictive bar and technology of preparing thereof.

Background technology

Rare earth ultra-magnetostriction material (GMM), the people such as United States Navy surface Weapons Laboratory CIark last century the seventies develop successful a kind of novel material, all incomparable magnetostrictive strain coefficient is high, energy density strong, adapt to the excellent technical characteristics such as wide frequency range, speed of response is fast, precision magnitude is high, unfailing performance is good to have any traditional magnetostriction materials.Rare earth ultra-magnetostriction material, since coming out, has been the forward position hot subject in new material technology field always, is the technical study field that countries in the world are all being paid close attention to.Through countries in the world scientific and technical personnel and manufacturing enterprise, make joint efforts, within short four times more than ten years, be developed rapidly perfect, the essential raw material that has now become the high-end technical products such as manufacturing electricity-acoustic transducer, electricity-machine transverter, professional sensor, special electronic devices and components, importance and influence power in countries in the world economic construction, national defense construction highlight day by day.

Take at present the west industrially developed country that the U.S. is representative, very advanced complete aspect the fundamental research of rare earth ultra-magnetostriction material, sizing has been mature on the whole aspect fabricating technology, aspect application device Development and Production, multi-field, be in full swing, becoming the leading motive force of production scientific research in the rare earth ultra-magnetostriction material technical field of countries in the world, left and right.But rare earth ultra-magnetostriction material still exists some shortcomings and weakness; Such as, aspect group material structure component, still continue to use the structure component of Tb-Dy-Fe ternary RE alloy, resistivity that raw material material self exists is little, high frequency characteristics is poor, fragility is high, loading capacity is low etc., and defect is not better solved; Aspect fabricating technology, still continue to use melt orientation freezing method and manufacture product, the configuration device that exists in technology of preparing is many, operational path long, handle control difficulty, unstable product quality, cost are crossed high defect and also better do not improved.However, the monopolistic strategy that west industrially developed country still relies on the intellecture properties such as patent, trade mark, standard and company of transnational group to carry out, in all many-sides such as technical study direction, product technology standard, specific equipment configurations, even, at aspects such as production marketing price, product application envrionment conditionss, all still bringing into play very important guiding or standardization role.

Developing of China's rare earth ultra-magnetostriction material started late, foundation is weak.Along with the kind quantity of China's high-end technology product constantly increases, China is also increasing to the quantity required of rare earth ultra-magnetostriction material.The market requirement is powerful pull under, participate in institution of higher learning, R&D institution and manufacturing enterprise that rare earth ultra-magnetostriction material develops recent years directly more and more, growth momentum is very violent, progressive very fast.

The Research progress of the domestic and international rare earth ultra-magnetostriction material technical field of tight tracking of the present invention, newest fruits are dynamically and development trend, on earnest analytical study Shortcomings and weakness basis, from selection group material structure component proportioning, research fabricating technology route, design configurations special technology equipment etc., relating to the main technical content that novel material develops starts with, adopt targetedly multiple innovative technology measure, form a kind of round bar shape powder of manufacturing out and control rareearth super magnetostrictive bar and technology of preparing thereof.

Summary of the invention

the technical problem that quasi-solution of the present invention is determined.

The present invention is according to magnetostrictive effect know-why, take polynary group of material proportioning, ultrasonic solid phase homogeneous be mixed, etc. static pressure press forming polarization, the successively innovative technology measure such as sintering sizing continuously, manufacture out a kind of powder smelting rareearth super magnetostrictive bar goods with excellent technical feature characteristics such as magnetostrictive strain coefficient are large, energy density strong, weave construction density is large, Curie point is high, mechanical and physical performance is good.

the technical scheme that technical solution problem of the present invention is taked.

The technical problem that the present invention solves, be achieved by the following technical programs: research and design goes out in iron (Fe), nickel (Ni), 3 kinds of magneticmetal material simple substance powder of cobalt (Co) the group material structure component that direct vast scale mixes lanthanum (La), 2 kinds of rare earth material simple substance powder of cerium (Ce), by polynary group of material proportioning, ultrasonic solid phase homogeneous are set, be mixed, etc. 5 relatively independent Technology operation units such as the polarization of static pressure press forming, successively sintering sizing continuously, commodity finishing and packing, be processed into a kind of round bar shape powder smelting rareearth super magnetostrictive bar goods.

Polynary group of described material proportioning operation unit, all should there is Magnetostrictive Properties according to the simple substance material of selecting, aboundresources, the cheap material characteristic that waits, the group material selection principles such as stronger mutual compensation incentive effect after assembly chemical combination, can have been given play to, choice for use has stronger magnetostrictive effect, fabulous mechanical and physical performance, the iron of higher density (Fe), nickel (Ni), 3 kinds of magneticmetal material simple substance metal-powders of cobalt (Co), choice for use has extremely strong magnetostrictive effect, higher density, the material characteristics such as larger resistivity, there is aboundresources, purify easily, the lanthanum of the resources advantages such as price is lower (La), 2 kinds of rare earth material simple substance powder of cerium (Ce), as group material structure component material.Each group material component proportioning share, by a gross weight of batch manufacturing powder smelting rareearth super magnetostrictive bar goods: 28～31 parts of iron (Fe); 14～16 parts, nickel (Ni); 9～8 parts of cobalts (Co); 27～25 parts of lanthanums (La); 22～20 parts of ceriums (Ce).The all need≤35 μ m of simple substance powder size of each group material component; Simple substance powder purity of each group material component all needs >=and 99.99%; All dirt adds up to total amount to need≤0.006%.

Research and design goes out direct vast scale in 3 kinds of magneticmetal material simple substance powder and mixes 2 kinds of rare earth material simple substance powder, because the 4f layer electronics of rare earth element has localization characteristics, accumulating in radius only has an appointment in 0.6～0.8 inner shell, be subject to outer 5s, the shielding of 5p and 6s electronics, make 4f layer electronic orbit and spin coupling effect, than rare earth central ion and large 1～2 order of magnitude of crystal field interaction that coordination ion produces, cause 4f electronic orbit to there is strong anisotropy around; When applying foreign field, can cause that lattice, along specific direction of magnetization, larger distortion occurs, and produces extremely strong magnetostrictive effect.Simultaneously, also because the molecular structure of rare earth element is all generally the chain crystal grain of growing up of arranging vertically, after recrystallize, be the long brilliant chain bridging arrangement state of dovetail shaped, there is stronger sagging resistance and creep properties preferably, after vast scale and other ferromagnetic metal material assembly chemical combination, there is extremely strong dispersion-strengthened action, can form film at its grain surface, performance " embedding effect ", form dispersoid particle, can there is with the inside magnetic domain of ferromagnetic metal material mutual compensation incentive effect, can effectively improve raising group material material capability, obtain high magnetostrictive strain coefficient and good mechanical and physical performance, can better solve all performance deficiencies that existing rare earth ultra-magnetostriction material exists aspect material quality.

The described ultrasonic solid phase homogeneous operation unit that is mixed, adopting a kind of advanced power ultrasonic homogeneous dispersion technology to be uniformly mixed to the innovation mixed technology that technology combines with traditional mechanical spraying, is a kind of by the multiple elemental metals powder ultrasonic solid phase homogeneous of the making multielement rare earth powdered alloy processes process that is mixed that is mixed.The ultrasonic solid phase homogeneous process operation technology that is mixed, by the multi-element metal powder ultrasonic solid phase homogeneous blender complete independently of research and design.

Multi-element metal powder ultrasonic solid phase homogeneous blender, is comprised of parts such as the tank that is mixed, powder spray feeder, board-like ultrasonic transducer, vacuum air pump, argon gas gas injection device, dispersed with stirring device, automatic control devices.The tank that is mixed, global design becomes totally-enclosed tapered structure of container, the tank that is mixed, the tank cover that is mixed, mounting bracket, consists of, and by mounting flange, is realized and being opened fast or closed operation; On the tank cover that is mixed, be mounted with the parts such as powder spray feeder, dispersed with stirring device, safety exhaust; On the tank that is mixed, be mounted with vacuum air pump, the parts such as total terminal box, argon gas gas injection device, discharge port and board-like ultrasonic transducer; Automatic control device is arranged on the outer appropriate location of the tank that is mixed.

Powder spray feeder, disperses first-class component to form by metal-powder hold-up vessel, powder high-pressure spray pump, powder, and 6 of design configurations are fixed on and are mixed on tank cover with 60 ° of sub-multiple angle positions of concentric(al) circles; By being alternately distributed principle, be respectively charged into the elemental metals powder that equivalent is divided into the iron metal powder of 2 parts and 4 kinds of other group material components.Powder spray feeder, can be by the elemental metals powder of whole 5 kinds of group material components, by mixed ratio, with the continuous spirt of dust cloud state, be mixed in tank simultaneously, make all groups of material component metal-powders accept solid phase dispersion homogeneous with dust cloud state and stir the operation that is mixed and process.

Board-like ultrasonic transducer, 3 groups of design configurations, are fixed on the outer wall of the tank that is mixed with 120 ° of sub-multiple angle positions, by total terminal box, are connected with the separated exciting ultrasonic generator in being arranged on automatic control device.Board-like ultrasonic transducer, the ultrasonic electric energy that separated exciting ultrasonic generator can be produced, converts to and has 42KHz frequency and 4.2W/cm ²the power ultrasonic of the sound intensity, penetrates from 3 directions the tank tank skin that is mixed simultaneously, and the dust cloud shape metal-powder radiation in the tank that is mixed is conducted.Because ultrasonic wave has extremely strong penetrativity and fabulous conductivity, in dust cloud shape pressed powder, conduct, can cause solia particle and enter high-frequency vibration state, produce and transmit huge energy, impel solia particle repeatedly constantly to antinode or node, to carry out displacement movement, produce displacement effect; Although the shift length of solia particle is little, the acceleration being directly proportional to ultrasonic frequency square is very big, even can reach several ten thousand times of universal gravity constant.Like this huge acceleration energy, is enough to cause that strong movement occurs all metal-powder particulates, the isostructuralism of colliding, break changes, and produces effective refinement, dispersion, homogeneous effect.

Dispersed with stirring device, is comprised of component such as variable-frequency motor, stir shaft, hock type dispersed with stirring dishes, is fixed on the central position of the tank cover that is mixed.Hock type dispersed with stirring dish, is fixed on stir shaft, is 2 groups of upper and lower bilayer structure arrangement forms; Every group has 2 dish-like dispersion chopping disks that are reverse installation, on the periphery and card of every dish-like dispersion chopping disk, is all mounted with 2 rows and disperses to cut hock.Dispersed with stirring device, carrying out dispersed with stirring while being mixed operation, due to the acting in conjunction of high speed rotating and special dish-like structure formation, in the card of 4 dish-like dispersion chopping disks, all can produce one extremely strong axial magnetism; The spirt dust cloud shape metal-powder in tank that is mixed, can by the card of 4 dish-like dispersion chopping disks, from axial relative direction, be sucked fast respectively, under the continuous action of follow-up supplementary extruding energy, dust cloud shape metal-powder can be respectively flows out to surrounding fast in the middle of the dish back of the body of dish-like dispersion chopping disk, collides after the tank tank skin that is mixed respectively both direction up and down and flows; Due to the structural shape of the tank that is mixed and the structural arrangement form acting in conjunction of 4 dish-like dispersion chopping disks, all dust cloud shape metal-powders in the tank that is mixed, can be sucked, flow out by 4 dish-like dispersion chopping disks respectively, form 4 and circulate route; The all dust cloud shape metal-powders in tank that are mixed, can different circulate route in fast rolling flow, obtain fully effectively dispersion, stirring, homogeneous, the operation that is mixed and process.Simultaneously, high speed rotary motion due to dispersed with stirring device, be arranged on the hock in every dish-like dispersion chopping disk periphery and card, can obtain the high frequency that metal powder granulates is clashed in high linear velocity and cutting, produce dynamic powers such as the extremely strong high speed shear power of metal powder granulates and centrifugal squeezes; This extremely strong dynamic potential energy, is enough to cause the metal powder granulates isostructuralism that is moved, collides, breaks and changes, and produces effective refinement, dispersion, homogeneous effect.

Automatic control device, is comprised of separated exciting ultrasonic generator and two-position controller two portions, and design is made and handled housing form, is fixed on separately on the outside correct position of blender; By the total terminal box of bundle conductor and blender, be connected.Separated exciting ultrasonic generator is partly comprised of four groundworks such as signal source, power magnification, input and output, controls, the digital waveform circuit devcie of employing based on micro-chip CAT89C51, ultrasonic electric energy is coupled on board-like ultrasonic transducer, reaches isolation and impedance matching.Two-position controller, is designed to have the automatic control functions such as Industry Control mcu programming, the on-the-spot online acquisition processing of signal, data calculating storage backup, keyboard input, instruction output, LED screen display; By bundle conductor, be connected with total terminal box, then be connected with the drive element such as the motor of each operation function parts, electric butterfly valve, frequency transformer, Mgs respectively by total terminal box.

The multi-element metal powder ultrasonic solid phase homogeneous blender special technology equipment of research and design, there is the several work functions such as injection, atomization, vibration, refinement, dispersion, homogeneous, stirring, mixing, can complete independently the ultrasonic solid phase homogeneous processes operation whole process that is mixed, can be disposable multiple elemental metals powder solid phase be mixed make have that component is controlled accurately, homogeneous dispersion fully, the multielement rare earth powdered alloy of the technical characteristic such as constituent element is evenly distributed, globule size standard, loose particles appropriateness.

Described operation unit such as polarization such as press forming such as static pressure such as grade, adopt a kind of innovation shaping Polarization technique that shaping dies is combined with static pressure hydraulic efficiency system, strong dc electric field system such as heating-cooling system, flexibilities, be a kind of by multielement rare earth powdered alloy compacting fine and close be shaping base substrate, what complete static magnetic field high temperature magnetic domain polarization orientation waits the static pressure press forming polarization process course of processing simultaneously.Deng static pressure press forming polarization process operation technique, by the bidirectional hydraulic shaping polarization machine complete independently of research and design.

Bidirectional hydraulic shaping polarization machine, is comprised of parts such as shaping dies, heating-cooling system, hydraulic efficiency system, strong dc electric field system, automatic maneuver control devices.Shaping dies, is separated the component such as sleeve pipe, mould housing, installation permanent seat, oil cylinder stroke stop means and is formed by shaping base substrate Xing Guan, rare earth alloy powder filler chamber, left and right movable pressing board, left and right closed cover, installation; By permanent seat is installed, be fixed on bed piece.The rare earth alloy powder filler chamber being formed by shaping base substrate type tube cavity, movable pressing board by design arrangement at two ends, left and right, be connected with left and right oil cylinder pressure head respectively, to multielement rare earth powdered alloy, apply bidirectional flexible hydrostatic pressure, complete the fine and close forming operation of compacting; Electric heating device, cooling water circulation sleeve pipe, mounting arrangements is being installed in the outer cavity forming between separation sleeve pipe and mould housing, to multielement rare earth powdered alloy and shaping base substrate, heat temperature raising is provided, cools and Heating temperature carried out effectively regulating and control operation; Strong dc coil, mounting arrangements, installing in the internal layer cavity forming between separation sleeve pipe and shaping base substrate type pipe, provides the operation of static magnetic field high temperature magnetic domain polarization orientation to shaping base substrate.

Heating-cooling system, be for multielement rare earth powdered alloy being carried out to the static pressure such as low temperature when suppressing fine and close forming operation or shaping base substrate being carried out to the operation of static magnetic field high temperature magnetic domain polarization orientation, heat temperature raising be provided, cool and Heating temperature is carried out effectively regulating the technical operation system of controlling.By component such as electric heating device, cooling water circulation sleeve pipe, cooling water circulating pump, water storage box, temperature sensor, measure monitor instrument, formed.Electric heating device, dividing into groups, interval, staggered mounting arrangements form, is fixed on mould housing, by bundle conductor, is connected with maneuver control device automatically; Cooling water circulation sleeve pipe, with around mounting arrangements form, is fixed on and installs on the outer wall of separating sleeve pipe, by water-in and water-out connecting water pipe, is connected respectively with cooling water circulating pump with water storage box; Temperature sensor, is fixed on the outer wall of shaping base substrate type pipe, by bundle conductor, is connected with automatic maneuver control device; Water storage box, mounting arrangements is on the other correct position of bed piece separately, and cooling water circulating pump is fixed on water storage box, by bundle conductor, is connected with automatic maneuver control device.Application of cold temperature is suppressed fine and close forming technique, when the static pressure such as multielement rare earth powdered alloy enforcement low temperature are suppressed to fine and close forming operation, by electric heating device, multielement rare earth powdered alloy is heated to 72～75 ℃, makes multielement rare earth powdered alloy can produce a kind of intensity of activation; There is this intensity of activation, can greatly improve surface atom magnetism and mechanical interlocking between powder particle, the intensity of base substrate of making to be shaped is effectively increased, also can greatly improve the mobility of powder particle, density and the homogeneous degree of base substrate of making to be shaped effectively improves, thereby produces the weave construction defects such as expansion, shrinkage porosite, crackle, bubble in the base substrate of effectively avoiding being shaped.Application high temperature magnetic domain polarization orientation technology, when shaping base substrate is implemented to the operation of static magnetic field high temperature magnetic domain polarization orientation, by electric heating device, shaping base substrate is heated to above after 395～400 ℃ of Curie point, steady temperature 15min, with the rate of temperature fall of 5 ℃/min, adjusts to the Heating temperature of shaping base substrate after 210～215 ℃ gradually, steady temperature 20min, with the rate of temperature fall of 3 ℃/min, gradually the Heating temperature of shaping base substrate is adjusted to after 100 ℃ again, closed strong dc electric field system; This temperature environment condition, in the base substrate that can make to be shaped, magnetic domain is easy to accept the magnetization of powerful static magnetic field, greatly improves magnetic moment polarization orientation ability, is conducive to obtain optimum polarization orientation effect.Heating-cooling system, by the automatic maneuver control device of design configurations, take to adjust the conduction time, the startup quantity that control electric heating device, adjust to control the engineering means such as the flow of water coolant in circulation sleeve pipe, flow velocity, can accurate adjustment control running technology parameters such as the Heating temperature of multielement rare earth powdered alloy or shaping base substrate, steady temperature time, temperature rates, and implement the hydraulic efficiency system of operation, the running technology parameter of strong dc electric field system keeps match synchronization simultaneously.

Hydraulic efficiency system, be for multielement rare earth powdered alloy being carried out to the static pressure such as low temperature when suppressing fine and close forming operation or shaping base substrate being carried out to the operation of static magnetic field high temperature magnetic domain polarization orientation, bidirectional flexible hydrostatic pressure be provided and the pressure operation of exerting pressure is carried out effectively regulating the technical operation system of controlling.By left oil cylinder pressure head, left oil cylinder, left oil pipe, form left to the fine and close operation unit of compacting, by left oil cylinder erection support, be fixed on bed piece, by left oil pipe, be connected with hydrauliccontroller, by left oil cylinder pressure head, be connected with the left movable pressing board of shaping dies; By right oil cylinder pressure head, right oil cylinder, right oil pipe, form right and suppress fine and close operation unit, by right oil cylinder erection support, be fixed on bed piece, by right oil pipe, be connected with hydrauliccontroller, by right oil cylinder pressure head, be connected with the right movable pressing board of shaping dies; Hydrauliccontroller, by hydraulic pressure components and parts such as hydraulic reservoir, geared oil pump, control valve, distribution valve, surplus valve, safety valve, Monitoring and Controlling instrument, formed, be fixed on separately on the other correct position of bed piece, by bundle conductor, be connected with automatic maneuver control device.Multielement rare earth powdered alloy compacting densification is become to shaping base substrate, require the pressure using must be able to make all powder particle all produce after brittle rupture, more again form neomorph; The running technology defects such as if the pressure using exists exert pressure insufficient pressure, the pressure inequality of exerting pressure, the time of exerting pressure is inadequate, decompress(ion) speed is too fast, just have part powder particle recoverable deformation only occurs, or just there is plastic deformation, also do not produce brittle rupture, pressure relief now, these powder particles that only occur recoverable deformation or plastic deformation just likely produce bounce-back or restore to the original state, the inner serious material hidden danger of quality such as expansion, shrinkage porosite, crackle, bubble that just likely therefore produces of neomorph.Therefore multielement rare earth powdered alloy is implemented to the fine and close forming operation of compacting, the enough powerful pressure and wait the static pressure mode of exerting pressure of exerting pressure must be provided, and can carry out effectively regulating control to running technology parameters such as pressure size, the travelling speed of exerting pressure, voltage stabilizing time, decompress(ion) speed.Hydraulic efficiency system, rely on left and right two oil cylinders of design configurations, all with 80Mpa powerful, be equal to operating pressure and all with the uniform and stable travelling speed of exerting pressure of 12mm/min, left and right two movable pressing boards that promote shaping dies from left and right both direction, can complete multielement rare earth powdered alloy is applied to flexible hydrostatic pressure from left and right both direction simultaneously; The circular tube wall of shaping base substrate type tube cavity can produce equal reactive force under this pressure-acting, from circumferential direction, exerts pressure to multielement rare earth powdered alloy simultaneously, can guarantee that each is to the pressure equalization equivalent of exerting pressure; Along with the continuous increase of this pressure, all can there is displacement and deformation by a relatively large margin in all multielement rare earth alloy powder particles successively, and occur successively to develop to plastic deformation from recoverable deformation, finally completes brittle rupture.In this process, the connecting forces between multielement rare earth alloy powder particle is greatly increased, and density is greatly improved, and volume is significantly dwindled; When the left and right movable pressing board of shaping dies is advanced to the spacing position of oil cylinder stroke of setting, left and right oil cylinder stops mobile, but still keeps original pressure of exerting pressure of 80MPa to continue to be applied on shaping base substrate, and keeps the longer voltage stabilizing time; At decompress(ion) sessions, take different rate of pressure reductions, successively decompression technique measure of the segmentation of different voltage stabilizing times, the static pressure such as complete and suppress fine and close forming operation whole process.Hydraulic efficiency system, by the automatic maneuver control device of configuration, the pressure techniques operating parameter of exerting pressure is carried out accurately effectively regulating and controlling, keep match synchronization with the heating-cooling system technical operation parameter of implementing operation simultaneously, can be disposable that the compacting of multielement rare earth powdered alloy is fine and close in having regulation geomery, pressurized general equilibrium, density distribution is even, tissue intensity is larger powder smelting rareearth super magnetostrictive bar shaping base substrate.

Strong dc electric field system, is when shaping base substrate being carried out to the operation of static magnetic field high temperature magnetic domain polarization orientation, higher static electric field intensity is provided and high temperature magnetic domain polarization orientation operation technique operating parameter is carried out effectively regulating the technical operation system of controlling.Strong dc electric field system, is comprised of component such as alternating current-direct current transformer, electronic stabilizer, volts DS automatic control device, strong dc coil, measurement monitoring instrument.Strong dc coil, is designed to the direct structural arrangement form around shaping base substrate type pipe, is fixed on shaping base substrate type pipe and installs in the internal layer cavity of separating between sleeve pipe, by bundle conductor, is connected with volts DS automatic control device; Alternating current-direct current transformer and electronic stabilizer connect fixing, and mounting arrangements, on the other correct position of bed piece, is connected with alternating-current power supply, volts DS automatic control device respectively by bundle conductor separately; Volts DS automatic control device, mounting arrangements is in automatic maneuver control device.Strong dc electric field system, take direct mounting arrangements strong dc coil on shaping base substrate type pipe outer wall, by the alternating current-direct current transformation voltage stabilizing power supply regulation device of configuration, stable high voltage galvanic current is provided, produce higher static electric field intensity, at shaping base substrate, keep, under enough powerful hydrostatic pressures, envrionment conditions higher than Curie point Heating temperature, completing shaping base substrate being carried out to static magnetic field high temperature magnetic domain polarization orientation technical operation.According to the requirement of static magnetic field high temperature magnetic domain polarization orientation Technology, when shaping base substrate maximum heating temperature reaches 395～400 ℃ higher than Curie point, make static electric field intensity reach 6kv/cm, and voltage stabilizing pressurize operation 15min; Keep synchronizeing with shaping base substrate rate of temperature fall, in shaping base substrate Heating temperature, adjust gradually and cool in 210～215 ℃, static electric field intensity is synchronously adjusted and risen to 8kv/cm gradually, then voltage stabilizing pressurize operation 20min; At shaping base substrate, cool in operation process, the voltage stabilizing pressurize all the time of static electric field intensity is at 8kv/cm, until shaping base substrate Heating temperature is closed electric field while dropping to 100 ℃.Strong dc electric field system, by adjusting the engineering measures such as DC voltage, conduction time, can control high temperature magnetic domain polarization orientation job run technical parameter by accurate adjustment, keep match synchronization with heating-cooling system, the hydraulic efficiency system running technology parameter of implementing operation simultaneously, can force the magnetic moment in shaping base substrate magnetic domain to carry out orderly orientations along static magnetic field direction, can obtain the best effect of static magnetic field high temperature magnetic domain polarization orientation operation.

Automatically maneuver control device, is designed to handle housing form, is fixed on separately on the other correct position of bed piece; Automatically maneuver control device has the automatic control functions such as Industry Control mcu programming, the on-the-spot online acquisition processing of signal, data calculating storage backup, keyboard input, instruction output, LED screen display; By bundle conductor, on the one hand transmit device with information acquisitions such as being arranged on sensor in operation field, measurement monitoring instrument and be connected, be connected with the driving part device such as the motor of each apparatus for work, pump, electric butterfly valve, Mgs on the one hand.

The bidirectional hydraulic shaping polarization machine special technology equipment of research and design, can multielement rare earth powdered alloy be carried out to the fine and close shapings of static pressure compacting such as low temperature and shaping base substrate is carried out to static magnetic field high temperature magnetic domain polarization orientation processes operation whole process by disposable complete independently, can greatly improve magnetostrictive strain coefficient and the Material texture technical feature of powder smelting rare earth magnetostriction rod material products, can simplify processes technical process, reduce specific equipment configuration quantity, reduce manufacturing cost.

Described sintering sizing operation unit successively continuously, adopting a kind of innovation sintering shaping technology that the bad body that is shaped is carried out successively continuously to low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering, anneal, is a kind of processes process of shaping base substrate being made to round bar shape powder smelting rareearth super magnetostrictive bar goods.Sintering setting process operation technique successively, has been equipped by special technologies such as low-temperature bake stove, intermediate sintering temperature stove, intermediate frequency high temperature sintering furnaces respectively continuously.

The sintering setting process operation technique successively continuously of research and design, the base substrate that can make to be shaped produces a kind of intensity of activation in the processes operation process such as the low-temperature bake carrying out successively, middle temperature presintering, intermediate frequency high temperature sintering, anneal.In shaping base substrate, there is this intensity of activation, just can impel the gravitational force between atoms on powder particle link surface in shaping base substrate to increase, connection ability improves, and can make generation between powder particle attract bonding reaction, dissolve and eliminate most of Elastic stress, most of gas and moisture content are got rid of in volatilization; Just can impel the atom amplitude of powder particle in shaping base substrate greatly to improve, allow abundant atom enter in atom sphere of gravitational action, by evaporation, diffusion, flow, the multiple migration form such as cohesion forms crystal grain boundary, and progressively inner mobile to powder particle, make the Distance Shortened between powder particle, porosity reduces, tissue density increases, structural volume is shunk, and makes internal stress obtain thoroughly eliminating and dissolving, and gas and moisture content obtain all getting rid of volatilization; Just the processing and manufacturing of shaping base substrate can be become and there are the powder smelting rareearth super magnetostrictive bar goods that weave construction does not have the outstanding technical feature characteristics such as defect, material density is fine and close evenly, mechanical and physical performance is stable, magnetostrictive effect is best.

Low-temperature bake, is to have the shaping base substrate of room temperature, puts in the low-temperature bake stove of argon gas protection, uses lesser temps to carry out baking process processing operation; Running technology parameter is: baking initial temperature is room temperature; baking temperature rise rate is 10 ℃/min; baking top temperature is 480 ℃ ﹙ ± 5 ℃ ﹚, and baking operation full time is 100min ﹙ ± 10min ﹚, and in low-temperature bake process, shielding gas argon flow amount is>=0.8m ³/ h.When the operation of low-temperature bake processes reached after whole baking activity duration of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 180 ℃ in stove, shaping base substrate is transferred in intermediate sintering temperature stove, carried out middle temperature pre-sintering process processing operation immediately.

Middle temperature presintering, is to be preheating to equal temperature and to have in the intermediate sintering temperature stove of argon gas protection having the shaping base substrate of more than 180 ℃ temperature, putting into, uses sufficient temp to carry out middle temperature pre-sintering process processing operation; Running technology parameter is: middle temperature presintering starting temperature is 180 ℃; presintering temperature rise rate is 15 ℃/min; presintering top temperature is 980 ℃ ﹙ ± 5 ℃ ﹚, and presintering operation full time is 150min ﹙ ± 10min ﹚, and in middle temperature presintering process, shielding gas argon flow amount is>=1.5m ³/ h.In the middle of warm pre-sintering process processing operation reach in design whole after the warm presintering activity duration, take power-off, die, open the measures such as fire door, dependence shaping base substrate naturally cooling method in stove is lowered the temperature; When temperature drops to 380 ℃ in stove, shaping base substrate is transferred in intermediate frequency high temperature sintering furnace, carried out intermediate frequency high-sintering process processing operation immediately.

Intermediate frequency high temperature sintering, is to have the shaping base substrate of more than 380 ℃ temperature, to put into and be preheating to equal temperature, has in the intermediate frequency high temperature sintering furnace of argon gas protection, uses comparatively high temps to carry out the high-sintering process processing operation of long period; Running technology parameter is: intermediate frequency high temperature sintering starting temperature is 380 ℃; Intermediate frequency high temperature sintering temperature rise rate is divided into 3 stages, the 1st stage: from 380 ℃, with the temperature rise rate continuous warming 10min of 17 ℃/min, make furnace temperature reach 550 ℃, steady temperature 10min; The 2nd stage: from 550 ℃, with the temperature rise rate continuous warming 30min of 10 ℃/min, make furnace temperature reach 850 ℃, steady temperature 15min; The 3rd stage: from 850 ℃, with the temperature rise rate continuous warming 25min of 15 ℃/min, make furnace temperature reach the top temperature controlling valu 1225 ℃ ﹙ ± 5 ℃ ﹚ of intermediate frequency high temperature sintering; On the temperature control line of this top temperature controlling valu, carry out the steady temperature sintering of long period, until reach intermediate frequency high temperature sintering operation full time 240min (± 20min); Shielding gas argon flow amount>=2m in intermediate frequency high-temperature sintering process ³/ h.When intermediate frequency high-sintering process processing operation reached after whole intermediate frequency high temperature sintering activity durations of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 380 ℃ in stove, again close immediately fire door, ventilation, energising, start the shaping base substrate in stove to carry out annealing treating process processing operation.

Anneal, is by the intermediate frequency high temperature sintering shaping base substrate with 380 ℃, in intermediate frequency high temperature sintering furnace, uses annealing temperature to carry out annealing treating process processing operation; Running technology parameter is: from 380(± 10 ℃), with the temperature rise rate continuous warming of 15 ℃/min, after 930 ℃ ﹙ ± 5 ℃ ﹚, stop heating up; In this temperature line, carry out steady temperature annealing, until reach annealing treating process processing operation full time 90min(± 10 min), in anneal process, shielding gas argon flow amount is>=0.8m ³/ h; After reaching anneal operation full time, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature, to room temperature, take out sintering molded article.

Described commodity finishing and packing operation unit is a kind of powder smelting rareearth super magnetostrictive bar goods to be carried out to the commercialization Technology course of processing.First, by the pneumatic sbot blasting machine of design configurations, the adhesive tape things such as the removing sizing that successively sintering sizing operation leaves at product surface continuously, burr, burning skin; Can improve product surface hardness, avoid transportation, keeping process to produce the defects such as cut, impression simultaneously.Secondly, the goods after clean and tidy cleaning are delivered to quality test department, by project, the program of product standard regulation, carry out quality of finished product check.Finally, to the qualified product through clean and tidy cleaning and outgoing check, by product standard regulation indicate, after the commercialization such as anticorrosion, collision protection, packing processes, warehouse-in is taken care of and is treated pin.

the advantage that the present invention has and the effect reaching.

(1), make full use of the huge resources advantage of China's rare earth reserves, the performance distinctive extremely strong magnetostrictive effect characteristic of rare earth element and dispersion-strengthened action and embedding effect, research and design goes out the polynary group of material proportioning innovative technology that directly mixes 2 kinds of rare earth material simple substance powder in 3 kinds of metallic substance simple substance powder with larger proportion, effectively improvement group material material quality, improve the technical features such as goods magnetostrictive strain coefficient, tensile strength, solve preferably existing material capability defect, expanded product application scope.

(2), make full use of the distinctive high frequency of power ultrasonic, high strength, high-energy produces strong mechanical vibration and displacement effect, making full use of mechanical spraying is uniformly mixed and produces great dispersing and mixing ability and high-speed impact, shear dynamic potential energy, research and design goes out the ultrasonic solid phase homogeneous innovative technology that is mixed, solved preferably multielement rare earth powdered alloy effective refinement powder particle granularity in solid phase is mixed, strengthening homogeneous dispersion degree, destruction is cleared up the technical barriers such as subparticle reunion adhesion energy, simplified preparation process, reduced manufacturing cost, improved production efficiency.

(3), research and design goes out shaping dies and heating-cooling system, hydraulic efficiency system, the innovative technology such as polarization such as press forming such as static pressure such as grade that strong dc electric field system combines, can be disposable by the fine and close shaping base substrate with definite shape and density that becomes of multielement rare earth powdered alloy compacting, and the base substrate that makes to be shaped is accepted the technical finesse of static magnetic field high temperature magnetic domain polarization orientation simultaneously, force the magnetic moment in shaping base substrate magnetic domain to carry out orderly orientations along static magnetic field direction, solved preferably the expansion very easily existing in shaping base substrate, shrinkage porosite, the material hidden danger such as crackle, can greatly improve magnetostrictive strain coefficient and goods technical feature quality.

(4), research and design goes out the innovation sintering shaping technology that shaping base substrate is carried out successively continuously to low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering, anneal, the gas that the volume of the base substrate that makes to be shaped obtains fully shrinking is closely knit, tissue intensity effectively improves, remaining internal stress obtains thoroughly dissolving eliminations, absorption and moisture content obtain all getting rid of that volatilization, polarization orientation obtain consolidating definite, magnetostrictive effect and mechanical and physical performance is maintained stable.

Accompanying drawing explanation

Accompanying drawing 1: powder smelting rareearth super magnetostrictive bar technology of preparing route schematic diagram.

Accompanying drawing 2: multi-element metal powder ultrasonic solid phase homogeneous blender structural principle schematic diagram.

Accompanying drawing 3: bidirectional hydraulic shaping polarization machine structural principle schematic diagram.

Embodiment

Technology of preparing and equipment special structural arrangement embodiment.

As shown in Figure 1, powder smelting rareearth super magnetostrictive bar and the technology of preparing thereof of research and design of the present invention, select to adopt by a batch gross weight for manufacturing powder smelting rareearth super magnetostrictive bar goods, 28～31 parts of iron (Fe), 14～16 parts, nickel (Ni), 9～8 parts of cobalts (Co), 27～25 parts of lanthanums (La), the group material structure component that cerium (Ce) is 22～20 parts; The all need≤35 μ m of simple substance powder size of each group material component, simple substance powder purity of each group material component all needs >=and 99.99%, all dirt adds up to total amount to need≤0.006%; By polynary group of material proportioning, ultrasonic solid phase homogeneous are set, be mixed, etc. 5 relatively independent Technology operation units such as the polarization of static pressure press forming, successively sintering sizing continuously, commodity finishing and packing, be processed into a kind of round bar shape powder smelting rareearth super magnetostrictive bar goods.

As shown in Figure 2, the described ultrasonic solid phase homogeneous Technology operation unit that is mixed, by multi-element metal powder ultrasonic solid phase homogeneous blender complete independently; Multi-element metal powder ultrasonic solid phase homogeneous blender, is comprised of parts such as the tank that is mixed, powder spray feeder (7), board-like ultrasonic transducer (5), vacuum air pump (6), argon gas gas injection device (13), dispersed with stirring device (4), automatic control devices (1).The tank that is mixed, global design becomes totally-enclosed tapered structure of container, the tank that is mixed (12), the tank cover (9) that is mixed, mounting bracket (15), consists of, and by mounting flange (10), is realized and being opened fast or closed operation.Upper at the tank cover (9) that is mixed, be mounted with the parts such as powder spray feeder (7), dispersed with stirring device (4), safety exhaust (8); Upper at the tank that is mixed (12), be mounted with vacuum air pump (6), the parts such as total terminal box (3), argon gas gas injection device (13), discharge port (14) and board-like ultrasonic transducer (5); Automatic control device (1) is arranged on the outer appropriate location of the tank that is mixed.

Powder spray feeder (7), disperses first-class component to form by metal-powder hold-up vessel, powder high-pressure spray pump, powder, and 6 of design configurations are fixed on and are mixed on tank cover (9) with 60 ° of sub-multiple angle positions of concentric(al) circles; By being alternately distributed principle, be respectively charged into the elemental metals powder that equivalent is divided into the iron metal powder of 2 parts and 4 kinds of other group material components.

Board-like ultrasonic transducer (5), 3 groups of design configurations, are fixed on the outer wall of the tank that is mixed (12) with 120 ° of sub-multiple angle positions, by total terminal box (3), are connected with the separated exciting ultrasonic generator in being arranged on automatic control device (1).Board-like ultrasonic transducer (5), the ultrasonic electric energy that separated exciting ultrasonic generator can be produced, converts to and has 42KHz frequency and 4.2W/cm ²the power ultrasonic of the sound intensity, from 3 directions, penetrate the tank tank skin that is mixed simultaneously, dust cloud shape metal-powder radiation in the tank that is mixed is conducted, cause powder particle and enter high-frequency vibration state, produce and transmit huge energy, impel powder particle repeatedly constantly to antinode or node, to carry out displacement movement, produce displacement effect; Make that strong movement occurs all metal-powder particulates, the isostructuralism of colliding, break changes, and produces effective refinement, dispersion, homogeneous effect.

Dispersed with stirring device (4), is comprised of component such as variable-frequency motor, stir shaft, hock type dispersed with stirring dishes, is fixed on the central position of tank cover (9) that are mixed.Hock type dispersed with stirring dish, is fixed on stir shaft, is 2 groups of upper and lower bilayer structure arrangement forms; Every group has 2 dish-like dispersion chopping disks (11) that are reverse installation, on the periphery and card of every dish-like dispersion chopping disk (11), is all mounted with 2 rows and disperses to cut hock.Dispersed with stirring device, carrying out dispersed with stirring while being mixed operation, due to the acting in conjunction of high speed rotating and special dish-like structure formation, in the card of 4 dish-like dispersion chopping disks (11), all can produce one extremely strong axial magnetism; The interior dust cloud shape metal-powder of the tank that is mixed, can by the card of dish-like dispersion chopping disk (11), from axial relative direction, be sucked fast respectively, under the continuous action of follow-up supplementary extruding energy, dust cloud shape metal-powder can be respectively flows out to surrounding fast in the middle of the dish back of the body of dish-like dispersion chopping disk (11), collides after the tank tank skin that is mixed respectively both direction up and down and flows; Due to the structural shape of the tank that is mixed (12) and the structural arrangement form acting in conjunction of 4 dish-like dispersion chopping disks (11), the all dust cloud shape metal-powders that are mixed in tank, can by 4 dish-like dispersion chopping disks (11), be sucked, flow out respectively, form 4 and circulate route; The all dust cloud shape metal-powders in tank that are mixed, can different circulate route in fast rolling flow, obtain fully effectively dispersion, stirring, homogeneous, the operation that is mixed and process.

As shown in Figure 3, the described static pressure press forming polarization process technical operation unit that waits, is completed by bidirectional hydraulic shaping polarization machine; Bidirectional hydraulic shaping polarization machine, is comprised of parts such as bed piece (16), shaping dies, heating-cooling system, hydraulic efficiency system, strong dc electric field system, automatic maneuver control devices (37).Shaping dies, is separated the component such as sleeve pipe (28), mould housing (25), installation permanent seat (19), oil cylinder stroke stop means and forms by shaping base substrate type pipe (32), rare earth alloy powder filler chamber (26), left and right movable pressing board (30,22), left and right closed cover (33,23), installation; By permanent seat (19) is installed, be fixed on bed piece (16).Installing in the outer cavity of separating formation between sleeve pipe (28) and mould housing (25), mounting arrangements has electric heating device (24), cooling water circulation sleeve pipe (27), installing in the internal layer cavity of separating formation between sleeve pipe (28) and shaping base substrate type pipe (32), mounting arrangements has strong dc coil (29).

Heating-cooling system, is comprised of component such as electric heating device (24), cooling water circulation sleeve pipe (27), cooling water circulating pump, water storage box, temperature sensor, measure monitor instrument.Electric heating device (24), dividing into groups, interval, staggered mounting arrangements form, is fixed on mould housing (25) upper, by bundle conductor, is connected with automatic maneuver control device (37); Cooling water circulation sleeve pipe (27), with around mounting arrangements form, is fixed on and installs on the outer wall of separating sleeve pipe (28), by water-in and water-out pipe connecting, is connected respectively with cooling water circulating pump with water storage box; Temperature sensor, is fixed on the outer wall of shaping base substrate type pipe (32), by bundle conductor, is connected with automatic maneuver control device (37).Water storage box, mounting arrangements is on the other correct position of bed piece (16) separately, and cooling water circulating pump is fixed on water storage box, by bundle conductor, is connected with automatic maneuver control device (37).When the static pressure such as multielement rare earth powdered alloy enforcement low temperature are suppressed to fine and close forming operation, by electric heating device (24), the multielement rare earth powdered alloy being seated in rare earth alloy powder filler chamber (26) is heated to 72～75 ℃, makes multielement rare earth powdered alloy produce a kind of intensity of activation; When shaping base substrate being implemented to the operation of static magnetic field high temperature magnetic domain polarization orientation, by adjustment control electric heating device (24) conduction time, start quantity and adjust engineering means such as controlling the flow of water coolant in circulation sleeve pipe (27), flow velocity, accurate adjustment is controlled running technology parameters such as the Heating temperature of shaping base substrate, steady temperature time, temperature rates, keeps match synchronization with the running technology parameter of implementing operation strong dc electric field system.

Hydraulic efficiency system, by left oil cylinder pressure head (31), left oil cylinder (34), left oil pipe (36), form left to the fine and close operation unit of compacting, by left oil cylinder erection support (35), be fixed on bed piece (16), by left oil pipe (36), be connected with hydrauliccontroller, by left oil cylinder pressure head (31), be connected with the left movable pressing board (30) of shaping dies; By right oil cylinder pressure head (21), right oil cylinder (20), right oil pipe (18), form right and suppress fine and close operation unit, by right oil cylinder erection support (17), be fixed on it machine tool (16), by right oil pipe (18), be connected with hydrauliccontroller, by right oil cylinder pressure head (21), be connected with the right movable pressing board (22) of shaping dies.Hydrauliccontroller, by hydraulic pressure components and parts such as hydraulic reservoir, geared oil pump, control valve, distribution valve, surplus valve, safety valve, Monitoring and Controlling instrument, formed, be fixed on separately on the other correct position of bed piece (16), by bundle conductor, be connected with automatic maneuver control device (37).The static pressure such as multielement rare earth powdered alloy enforcement low temperature are being suppressed in fine and close forming technology technological processes, rely on left and right two oil cylinders (34,20) of design configurations, all with 80Mpa powerful, be equal to operating pressure and all with the uniform and stable travelling speed of exerting pressure of 12mm/min, from left and right both direction, promote left and right two movable pressing boards (30,22) of shaping dies, to being seated in the multielement rare earth powdered alloy in rare earth alloy powder filler chamber (26), from left and right both direction, apply flexible hydrostatic pressure simultaneously; The circular tube wall of shaping base substrate type pipe (32) inner chamber can produce equal reactive force under this pressure-acting, from circumferential direction, to multielement rare earth powdered alloy, exerts pressure simultaneously, makes all directions pressure equalization equivalent of exerting pressure; When the left and right movable pressing board (30,22) of shaping dies is advanced to the spacing position of oil cylinder stroke of setting, left and right oil cylinder (34,20) stops mobile, but still can keep original pressure of exerting pressure of 80MPa to continue to be applied on shaping base substrate, and keep the longer voltage stabilizing time.At decompress(ion) sessions, different rate of pressure reductions, successively decompression technique measure of the segmentation of different voltage stabilizing times are taked in design, the static pressure such as complete and suppress fine and close forming operation whole process.

Strong dc electric field system, is comprised of component such as alternating current-direct current transformer, electronic stabilizer, volts DS automatic control device, strong dc coil (29), measurement monitoring instrument.Strong dc coil (29), be designed to directly the structural arrangement form around shaping base substrate type pipe (32), be fixed on shaping base substrate type pipe (32) and install in the internal layer cavity of separating between sleeve pipe (28), by bundle conductor, being connected with volts DS automatic control device; Alternating current-direct current transformer and electronic stabilizer connect fixing, and mounting arrangements, on the other correct position of bed piece (16), is connected with alternating-current power supply, volts DS automatic control device respectively by bundle conductor separately; Volts DS automatic control device, mounting arrangements is in automatic maneuver control device (37).When shaping base substrate being implemented to the operation of static magnetic field high temperature magnetic domain polarization orientation Technology, by adjusting the engineering measures such as DC voltage, conduction time, can control the job run technical parameters such as static electric field intensity, pressurize voltage stabilizing activity duration by accurate adjustment, keep match synchronization with envrionment conditions factors such as implementing the heating-cooling system of operation, Heating temperature, heating steady warm time, the temperature rate that hydraulic efficiency system forms, the pressure of exerting pressure, voltage stabilizing time, force the magnetic moment in shaping base substrate magnetic domain to carry out orderly orientations along static magnetic field direction.

As shown in Figure 1; described sintering setting process technical operation unit successively continuously; take shaping base substrate to carry out continuously successively the sintering setting process processing operation of low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering, anneal, by design configurations, had the special technologies such as low-temperature bake stove, intermediate sintering temperature stove, intermediate frequency high temperature sintering furnace of argon gas protection to equip.

Low-temperature bake, is to have the shaping base substrate of room temperature, puts in the low-temperature bake stove of argon gas protection, uses lesser temps to carry out baking process processing operation process; Running technology parameter is: low-temperature bake initial temperature is room temperature; baking temperature rise rate is 10 ℃/min; baking top temperature is 480 ℃ ﹙ ± 5 ℃ ﹚, and baking operation full time is 100min ﹙ ± 10min ﹚, and in low-temperature bake process, shielding gas argon flow amount is>=0.8m ³/ h.When the operation of low-temperature bake processes reached after whole baking activity duration of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 180 ℃ in stove, shaping base substrate is transferred in intermediate sintering temperature stove, carried out middle temperature pre-sintering process processing operation immediately.

Middle temperature presintering, is to be preheating to equal temperature and to have in the intermediate sintering temperature stove of argon gas protection having the shaping base substrate of more than 180 ℃ temperature, putting into, uses sufficient temp to carry out middle temperature pre-sintering process processing operation process; Running technology parameter is: middle temperature presintering starting temperature is 180 ℃; presintering temperature rise rate is 15 ℃/min; presintering top temperature is 980 ℃ ﹙ ± 5 ℃ ﹚, and presintering operation full time is 150min ﹙ ± 10min ﹚, and in middle temperature presintering process, shielding gas argon flow amount is>=1.5m ³/ h.In the middle of warm pre-sintering process processing operation reach in design whole after the warm presintering activity duration, take power-off, die, open the measures such as fire door, dependence shaping base substrate naturally cooling method in stove is lowered the temperature; When temperature drops to 380 ℃ in stove, shaping base substrate is transferred in intermediate frequency high temperature sintering furnace, carried out intermediate frequency high-sintering process processing operation immediately.

Intermediate frequency high temperature sintering, is to have the shaping base substrate of more than 380 ℃ temperature, puts into and is preheating to equal temperature, has in the intermediate frequency high temperature sintering furnace of argon gas protection, uses comparatively high temps to carry out the high-sintering process processing operation process of long period; Running technology parameter is: intermediate frequency high temperature sintering starting temperature is 380 ℃; Intermediate frequency high temperature sintering temperature rise rate is divided into 3 stages, the 1st stage: from 380 ℃, with the temperature rise rate continuous warming 10min of 17 ℃/min, make furnace temperature reach 550 ℃, steady temperature 10min; The 2nd stage: from 550 ℃, with the temperature rise rate continuous warming 30min of 10 ℃/min, make furnace temperature reach 850 ℃, steady temperature 15min; The 3rd stage: from 850 ℃, with the temperature rise rate continuous warming 25min of 15 ℃/min, make furnace temperature reach the top temperature controlling valu 1225 ℃ ﹙ ± 5 ℃ ﹚ of intermediate frequency high temperature sintering; On the temperature control line of this top temperature controlling valu, carry out the steady temperature sintering of long period, until reach intermediate frequency high temperature sintering operation full time 240min (± 20min); Shielding gas argon flow amount>=2m in intermediate frequency high-temperature sintering process ³/ h.When intermediate frequency high-sintering process processing operation reached after whole intermediate frequency high temperature sintering activity durations of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 380 ℃ in stove, again close immediately fire door, ventilation, energising, start the shaping base substrate in stove to carry out annealing treating process processing operation.

Anneal, is by the intermediate frequency high temperature sintering shaping base substrate with 380 ℃, in intermediate frequency high temperature sintering furnace, uses annealing temperature to carry out annealing treating process processing operation process; Running technology parameter is: anneal starting temperature is 380(± 10 ℃), with the temperature rise rate continuous warming of 15 ℃/min, after 930 ℃ ﹙ ± 5 ℃ ﹚, stop heating up; In this temperature line, carry out steady temperature annealing, until complete annealing treating process processing operation full time 90min(± 10 min), shielding gas argon flow amount>=0.8m in annealing process ³/ h.Until annealing process processing operation, reach after the anneal operation full time of design, then take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; Until drop to after room temperature, take out the powder smelting rareearth super magnetostrictive bar goods of sintering sizing.

As shown in Figure 1, described commodity finishing and packing Technology operation unit, be to powder smelting rareearth super magnetostrictive bar goods neatly clear up, the commercialization processes process such as sign, anticorrosion, collision protection, packing.

Technology operation embodiment.

Powder smelting rareearth super magnetostrictive bar and the technology of preparing thereof of research and design of the present invention, by polynary group of material proportioning, ultrasonic solid phase homogeneous are set, be mixed, etc. 5 relatively independent Technology operation units such as the polarization of static pressure press forming, successively sintering sizing continuously, commodity finishing and packing, be processed into a kind of round bar shape powder smelting rareearth super magnetostrictive bar goods.The embodiment of each Technology operation unit is:

Polynary group of material proportioning operation unit.

---according to manufacturing the technical requirements of powder smelting rareearth super magnetostrictive bar product producing process file to polynary group of material proportioning, according to production schedules arrangement, prepare in proportion sufficient each group material component simple substance powder that meets the technological standard requirements such as granularity, purity, grade standby.

The ultrasonic solid phase homogeneous operation unit that is mixed.

---according to the requirement of polynary group of material proportion technique, batch gross weight of manufacturing powder smelting rareearth super magnetostrictive bar goods of take is radix, take into full account the factors such as scaling loss in preparation process, consumption, by the filling rate of multi-element metal powder ultrasonic solid phase homogeneous blender useful volume≤58% of configuration, accurately calculate the concrete weight that each group material component simple substance powder feeds intake in this batch of manufacturing.

---according to calculation result, by the electronics automatic Weighing device of configuration, each group material component simple substance powder is carried out respectively to Weighing, concrete weight metering is all accurate to gram; Iron metal powder equivalent is divided into 2 parts, with other 4 kinds of metal-powders by being alternately distributed principle, being respectively charged in 6 the powder spray feeders (7) that are arranged on multi-element metal powder ultrasonic solid phase homogeneous blender.

---start the vacuum air pump (6) on multi-element metal powder ultrasonic solid phase homogeneous blender, extract the air in the tank that is mixed out; Treat that in tank, vacuum tightness reaches 12 * 10 ^-3during Pa, close vacuum air pump (6).

---start immediately argon gas gas injection device (13), in the tank that is mixed, inject inert shielding gas argon gas; Treat that in tank, argon gas gas injection rate reaches 0.12m ³/ m ³time, close argon gas gas injection device (13).

---start immediately 6 powder spray feeders (7) simultaneously, 5 kinds of simple substance powder are injected in the tank that is mixed with the even continuous spraying of dust cloud state by mixed ratio simultaneously; All the material spray time is controlled in 40～50min and completes, and closes powder spray feeder (7) after fulfiling assignment.

---when starting powder spray feeder (7), start dispersed with stirring device (4); Make it with the rotating speed high speed rotating of 1200r/min, drive spray into the dust cloud sprills in the tank that is mixed continuously fast rolling flow, accept the shock cutting of dish-like dispersion chopping disk (11) hock simultaneously and disperse to stir the operation that is mixed.

---after closing powder spray feeder (7) 10～12min, by the adjustment of rotational speed of dispersed with stirring device (4), be 800r/min; Meanwhile start ultrasonic generator, ultrasonic electric energy is coupled to 3 groups of board-like ultrasonic transducers (5) upper, send and there is 42KH _zfrequency and 4.2w/cm ²the power ultrasonic of the sound intensity, the dust cloud sprills radiation conduction in simultaneously from 3 directions to the tank that is mixed, causes powder particle and enters high-frequency vibration state, makes powder particle produce displacement, the isostructuralism of colliding, break changes; The ultrasonic radiation time reaches after 25～28min, closes ultrasonic generator.

---after ultrasonic radiation stops, dispersed with stirring device (7) continues after rotating speed with 800r/min moves 30min continuously to cut out dispersed with stirring device (7), stops operation.After the 15min that stops operation, open discharge port (14), take out the multielement rare earth powdered alloy of making; Pack tube for feed sealing into, temporary stand-by.

Deng static pressure press forming polarization operation unit.

---according to concrete technical qualification such as the density of manufacturing powder smelting rareearth super magnetostrictive bar goods, net weight, shape, sizes, take into full account the factors such as the consumption of multielement rare earth powdered alloy in press forming and sintering type-approval process, scaling loss, shaping porosity, sintering shrinkage, accurately calculate the concrete weight of multielement rare earth powdered alloy that this waits static pressure press forming polarization operation to load.

---according to calculation result, the electronics automatic Weighing device by design configurations, carries out Weighing to multielement rare earth powdered alloy; Then pack on the bidirectional hydraulic shaping polarization machine of configuration in the rare earth alloy powder filler chamber (26) in shaping dies; After filling, sealing shaping dies.

---start the electric heating device (24) in heating-cooling system on bidirectional hydraulic shaping polarization machine, the multielement rare earth powdered alloy packing in shaping dies is heated to 72～75 ℃, and this temperature-stable is retained to and suppresses densification for shaping base substrate.

---start subsequently the hydraulic efficiency system of bidirectional hydraulic shaping polarization machine, make left and right two oil cylinders (34,20) can be with the stable and uniform working speed of 12mm/min and the operating pressure of 80MPa, pressure and speed from left and right both direction to be equal to, the left and right movable pressing board (30,22) that promotes uniformly and stably shaping dies, applies bidirectional flexible hydrostatic pressure to multielement rare earth powdered alloy; Form the circular tube wall of shaping base substrate type pipe (32) inner chamber of rare earth alloy powder filler chamber (26), under this pressure-acting, produce equal reactive force, at circumferential direction, to multielement rare earth powdered alloy, exert pressure, make multielement rare earth powdered alloy accept the fine and close compacting pressure general equilibrium of compacting from all directions simultaneously.

---the left and right movable pressing board (30,22) of shaping dies is advanced to behind the spacing position of oil cylinder stroke of design, stops mobile; But left and right oil cylinder (34,20) still keeps the original operating pressure of 80MPa, continues to be applied on multielement rare earth powdered alloy.Now, the multielement rare earth powdered alloy being seated in rare earth alloy powder filler chamber (26) has had displacement and deformation by a relatively large margin, and all powder particle all progressively completes from recoverable deformation and develops to plastic deformation, finally realizes brittle rupture; In this process, the connection ability between powder particle progressively strengthens, and volume progressively dwindles, and formation has the shaping base substrate of certain specification size, certain density, some strength.

---bidirectional hydraulic shaping polarization machine keeps after voltage stabilizing 40min under this pressure, adjust the Heating temperature of heating-cooling system, shaping base substrate in rare earth alloy powder filler chamber (26) is heated to above after 395～400 ℃ of Curie point, start immediately strong dc electric field system, start shaping base substrate to carry out the operation of static magnetic field high temperature magnetic domain polarization orientation Technology:

First, by tetanic electric field system, static electric field intensity is adjusted to 6kv/cm (± 10v/cm), start shaping base substrate to carry out polarization orientation operation, under this strength of electric field condition, the activity duration keeps 15min(± 2min).Then, by heating-cooling system, by the rate of temperature fall with 5 ℃/min to the Heating temperature of shaping base substrate, adjust to gradually 210～215 ℃; Synchronize with adjustment Heating temperature, by strong dc electric field system, static electric field intensity is adjusted to 8kv/cm(± 15v/cm gradually); After Heating temperature and strength of electric field are all adjusted to the right place, under this Heating temperature and strength of electric field envrionment conditions, shaping base substrate is carried out to the activity duration of polarization orientation, keep 20min(± 2min).Finally, by heating-cooling system, by the rate of temperature fall with 3 ℃/min to the Heating temperature of shaping base substrate, carry out cooling down; In this process, strength of electric field remains and is stabilized in 8kv/cm (± 15v/cm); When shaping base substrate cooling down to 100 ℃, close strong dc electric field system, withdraw from externally-applied magnetic field.After this, the rate of temperature fall of the bad body that is shaped is thrown away and remained on 3 ℃/min, until drop to room temperature.

---shaping base substrate cooling down, after room temperature, starts to carry out successively decompress(ion) discharging operation of segmentation by hydraulic efficiency system:

For the first time, the rate of pressure reduction with 0.5MPa/min, is decompressed to 60MPa from 80MPa; Voltage stabilizing 20min under this pressure.For the second time, the rate of pressure reduction with 0.8MPa/min, is decompressed to 20MPa from 60MPa; Voltage stabilizing 15min under this pressure.For the third time, with the rate of pressure reduction of 1MPa/min, from 20MPa, directly reduce to and remove whole pressure.

---after removing whole pressure 10min, open shaping dies, the polarize powder smelting rareearth super magnetostrictive bar shaping base substrate of operation of static pressure press forming such as has taken out; After interim packing is processed, temporary stand-by.

Sintering sizing operation unit successively continuously.

---by powder smelting rareearth super magnetostrictive bar shaping base substrate, put in the low-temperature bake stove with argon gas atmosphere protection, use lesser temps to carry out low-temperature bake operation to shaping base substrate.The initial temperature of low-temperature bake is room temperature, and temperature rise rate remains on 10 ℃/min, and the highest storing temperature is controlled at 480 ℃ (± 5 ℃); All baking time is controlled at 100min (± 10 min), remain on>=0.8m of shielding gas argon flow amount in bake process ³/ h.When low-temperature bake reaches after whole baking times, take power-off, die, open fire door measure, by shaping base substrate naturally cooling method in stove, lower the temperature; When temperature is down to 180 ℃ in stove, shaping base substrate is transferred in intermediate sintering temperature stove, proceeded middle temperature presintering operation immediately.

---by thering is the shaping base substrate of more than 180 ℃ temperature, putting into, be preheating in the intermediate sintering temperature stove that equal temperature has argon gas atmosphere protection, use sufficient temp to carry out middle temperature presintering operation.Middle temperature presintering temperature rise rate remains on 15 ℃/min; senior middle school temperature pre-sintering temperature is controlled at 980 ℃ (± 5 ℃); all, the warm presintering time is controlled at 150min (± 10 min), remain on>=1.5m of shielding gas argon flow amount in middle temperature presintering process ³/ h.Central warm presintering reached after whole presintering time, taked power-off, died, opens fire door measure, by shaping base substrate naturally cooling method in stove, lowered the temperature; When temperature is down to 380 ℃ in stove, middle temperature presintering shaping base substrate is transferred in intermediate frequency high temperature sintering furnace, carried out the operation of intermediate frequency high temperature sintering immediately.

---by thering is the shaping base substrate of more than 380 ℃ temperature, putting into, be preheating in the intermediate frequency high temperature sintering furnace that equal temperature has argon gas atmosphere protection, use comparatively high temps to carry out the intermediate frequency high temperature sintering operation of long period.The temperature rise rate of intermediate frequency high temperature sintering operation is divided into 3 stages: in the 1st stage, from 380 ℃, with the temperature rise rate continuous warming 10min of 17 ℃/min, make furnace temperature reach 550 ℃, steady warm 10 min; In the 2nd stage, from 550 ℃, with temperature rise rate continuous warming 30 min of 10 ℃/min, make furnace temperature reach 850 ℃, steady warm 15 min; The 3rd stage, from 850 ℃, temperature rise rate continuous warming 25 min with 15 ℃/min, make furnace temperature reach 1225 ℃ of the top temperature controlling valus (± 5 ℃) of intermediate frequency high temperature sintering operation, on this top temperature controlling valu temperature control line, carry out the steady temperature sintering of long period, make whole sintering times of intermediate frequency high temperature sintering operation reach 240min (± 20 min); Remain on>=2m of shielding gas argon flow amount in intermediate frequency high-temperature sintering process ³/ h.When the operation of intermediate frequency high temperature sintering reached after whole intermediate frequency high temperature sintering time, take power-off, die, open fire door measure, by shaping base substrate naturally cooling method in stove, lower the temperature.

---when temperature is down to 380 ℃ (± 10 ℃) in stove, again close fire door, energising, ventilation, start shaping base substrate to carry out anneal operation.First, from 380 ℃, after the temperature rise rate continuous warming to 930 ℃ (± 5 ℃) with 15 ℃/min, stop heating up; On this temperature control line, carry out steady temperature annealing 90 min(± 10 min); Remain on>=0.8m of shielding gas argon flow amount in anneal process ³/ h.Until the furnace annealing temperature control time, reach after the steady temperature annealing time of regulation, take power-off, die, open fire door measure, by shaping base substrate naturally cooling method in stove, lower the temperature.

---until temperature in stove, be down to after normal temperature, take out the powder smelting rareearth super magnetostrictive bar goods of sintering sizing.

Commodity finishing and packing operation unit.

---by the pneumatic sbot blasting machine of design configurations, the adhesive tape things such as the sizing of removing powder smelting rareearth super magnetostrictive bar product surface, burr, burning skin; Improve product surface hardness simultaneously, avoid transportation, keeping process to produce the defects such as cut, impression.

---the goods after clean and tidy cleaning are delivered to quality test department, by project, the program of product standard regulation, carry out the check of goods outgoing.

---to the qualified product through clean and tidy cleaning and outgoing check, by product standard regulation indicate, after the commercialization such as anticorrosion, collision protection, packing processes, warehouse-in is taken care of and is treated pin.

Claims (4)

1. a powder smelting rareearth super magnetostrictive bar and technology of preparing thereof, it is characterized in that: this powder smelting rareearth super magnetostrictive bar and technology of preparing thereof, the group material structure component adopting, by a batch gross weight for manufacturing powder smelting rareearth super magnetostrictive bar goods, 28～31 parts of iron (Fe), 14～16 parts, nickel (Ni), 9～8 parts of cobalts (Co), 27～25 parts of lanthanums (La), 22～20 parts of ceriums (Ce); By polynary group of material proportioning, ultrasonic solid phase homogeneous are set, be mixed, etc. 5 relatively independent Technology operation units such as the polarization of static pressure press forming, successively sintering sizing continuously, commodity finishing and packing be processed into.

2. a kind of powder smelting rareearth super magnetostrictive bar according to claim 1 and technology of preparing thereof, is characterized in that: the described ultrasonic solid phase homogeneous Technology operation unit that is mixed, by multi-element metal powder ultrasonic solid phase homogeneous blender complete independently; Multi-element metal powder ultrasonic solid phase homogeneous blender, comprises the tank that is mixed, powder spray feeder (7), board-like ultrasonic transducer (5), vacuum air pump (6), argon gas gas injection device (13), dispersed with stirring device (4), automatic control device (1); The described tank that is mixed, global design becomes totally-enclosed tapered structure of container, the tank that is mixed (12), the tank cover (9) that is mixed, mounting bracket (15), mounting flange (10), consists of; On the tank cover (9) that is mixed, be mounted with powder spray feeder (7), dispersed with stirring device (4), safety exhaust (8), on the tank that is mixed (12), be mounted with vacuum air pump (6), total terminal box (3), argon gas gas injection device (13), discharge port (14), board-like ultrasonic transducer (5), automatic control device (1) is arranged on the outer appropriate location of the tank that is mixed; Described powder spray feeder (7), by metal-powder hold-up vessel, powder high-pressure spray pump, powder dispersing head, formed, 6 of design configurations, with 60 ° of sub-multiple angle positions of concentric(al) circles, be fixed on the tank cover (9) that is mixed upper, by being alternately distributed principle, be respectively charged into iron metal powder and the 4 kinds of simple substance powder of organizing material components that equivalent is divided into 2 parts; Described board-like ultrasonic transducer (5), 3 groups of design configurations, with 120 ° of sub-multiple angle positions, be fixed on the outer wall of the tank that is mixed (12), by total terminal box (3), be connected with the separated exciting ultrasonic generator in being arranged on automatic control device (1); Described dispersed with stirring device (4), is comprised of variable-frequency motor, stir shaft, hock type dispersed with stirring dish, is fixed on the central position of tank cover (9) that are mixed; Hock type dispersed with stirring dish, be fixed on stir shaft, be 2 groups of upper and lower bilayer structure arrangement forms, every group has 2 dish-like dispersion chopping disks (11) that are reverse installation, on the periphery and card of every dish-like dispersion chopping disk (11), be all mounted with 2 rows and disperse to cut hock.

3. a kind of powder smelting rareearth super magnetostrictive bar according to claim 1 and technology of preparing thereof, is characterized in that: described static pressure press forming polarization process technical operation unit such as grade, is completed by bidirectional hydraulic shaping polarization machine; Bidirectional hydraulic shaping polarization machine, comprises bed piece (16), shaping dies, heating-cooling system, hydraulic efficiency system, strong dc electric field system, automatic maneuver control device (37); Described shaping dies, by shaping base substrate type pipe (32), rare earth alloy powder filler chamber (26), left and right movable pressing board (30,22), left and right closed cover (33,23), installation separation sleeve pipe (28), mould housing (25), installation permanent seat (19), oil cylinder stroke stop means, formed, by permanent seat (19) is installed, be fixed on bed piece (16); Installing in the outer cavity of separating formation between sleeve pipe (28) and mould housing (25), mounting arrangements has electric heating device (24), cooling water circulation sleeve pipe (27), installing in the internal layer cavity of separating formation between sleeve pipe (28) and shaping base substrate type pipe (32), mounting arrangements has strong dc coil (29); Described heating-cooling system, is comprised of electric heating device (24), cooling water circulation sleeve pipe (27), cooling water circulating pump, water storage box, temperature sensor, measure monitor instrument; Electric heating device (24), dividing into groups, interval, be staggered installation of arrangement form, is fixed on mould housing (25) upper, by bundle conductor, is connected with automatic maneuver control device (37); Cooling water circulation sleeve pipe (27), with around mounting arrangements form, is fixed on and installs on the outer wall of separating sleeve pipe (28), by water-in and water-out connecting water pipe, is connected respectively with cooling water circulating pump with water storage box; Temperature sensor, is fixed on the outer wall of shaping base substrate type pipe (32), by bundle conductor, is connected with automatic maneuver control device (37); Water storage box, mounting arrangements is on the other correct position of bed piece (16) separately, and cooling water circulating pump is fixed on water storage box, by bundle conductor, is connected with automatic maneuver control device (37); Described hydraulic efficiency system, by left oil cylinder pressure head (31), left oil cylinder (34), left oil pipe (36), form left to the fine and close operation unit of compacting, by left oil cylinder erection support (35), be fixed on bed piece (16), by left oil pipe (36), be connected with hydrauliccontroller, by left oil cylinder pressure head (31), be connected with the left movable pressing board (30) of shaping dies; By right oil cylinder pressure head (21), right oil cylinder (20), right oil pipe (18), form right and suppress fine and close operation unit, by right oil cylinder erection support (17), be fixed on it machine tool (16), by right oil pipe (18), be connected with hydrauliccontroller, by right oil cylinder pressure head (21), be connected with the right movable pressing board (22) of shaping dies; Hydrauliccontroller, by hydraulic reservoir, geared oil pump, control valve, distribution valve, surplus valve, safety valve, Monitoring and Controlling instrument, formed, be fixed on separately on the other correct position of bed piece (16), by bundle conductor, be connected with automatic maneuver control device (37); Described strong dc electric field system, is comprised of alternating current-direct current transformer, electronic stabilizer, volts DS automatic control device, strong dc coil (29), measurement monitoring instrument; Strong dc coil (29), be designed to directly the structural arrangement form around shaping base substrate type pipe (32), be fixed on shaping base substrate type pipe (32) and install in the internal layer cavity of separating between sleeve pipe (28), by bundle conductor, being connected with volts DS automatic control device; Alternating current-direct current transformer and electronic stabilizer connect fixing, and mounting arrangements, on the other correct position of bed piece (16), is connected with alternating-current power supply, volts DS automatic control device respectively by bundle conductor separately; Volts DS automatic control device, mounting arrangements is in automatic maneuver control device (37).

4. a kind of powder smelting rareearth super magnetostrictive bar according to claim 1 and technology of preparing thereof, it is characterized in that: described sintering setting process technical operation unit successively continuously, by having low-temperature bake stove, intermediate sintering temperature stove, the intermediate frequency high temperature sintering furnace of argon gas protection to complete; The running technology parameter of low-temperature bake processes operation is: baking initial temperature is room temperature; baking temperature rise rate is 10 ℃/min; baking top temperature is 480 ℃ ﹙ ± 5 ℃ ﹚; baking operation full time is 100min ﹙ ± 10min ﹚, and in low-temperature bake process, shielding gas argon flow amount is>=0.8m ³/ h; When the operation of low-temperature bake processes reached after whole baking activity duration of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 180 ℃ in stove, shaping base substrate is transferred in intermediate sintering temperature stove, carried out middle temperature pre-sintering process processing operation immediately; The running technology parameter of middle temperature pre-sintering process processing operation is: middle temperature presintering starting temperature is 180 ℃; presintering temperature rise rate is 15 ℃/min; presintering top temperature is 980 ℃ ﹙ ± 5 ℃ ﹚; presintering operation full time is 150min ﹙ ± 10min ﹚, and in middle temperature presintering process, shielding gas argon flow amount is>=1.5m ³/ h; In the middle of warm pre-sintering process processing operation reach in design whole after the warm presintering activity duration, take power-off, die, open the measures such as fire door, dependence shaping base substrate naturally cooling method in stove is lowered the temperature; When temperature drops to 380 ℃ in stove, shaping base substrate is transferred in intermediate frequency high temperature sintering furnace, carried out intermediate frequency high-sintering process processing operation immediately; The running technology parameter of intermediate frequency high-sintering process processing operation is: intermediate frequency high temperature sintering starting temperature is 380 ℃; Intermediate frequency high temperature sintering temperature rise rate is divided into 3 stages: in the 1st stage, from 380 ℃, with the temperature rise rate continuous warming 10min of 17 ℃/min, make furnace temperature reach 550 ℃, steady temperature 10min; In the 2nd stage, from 550 ℃, with the temperature rise rate continuous warming 30min of 10 ℃/min, make furnace temperature reach 850 ℃, steady temperature 15min; The 3rd stage; from 850 ℃; temperature rise rate continuous warming 25min with 15 ℃/min; make furnace temperature reach the top temperature controlling valu 1225 ℃ ﹙ ± 5 ℃ ﹚ of intermediate frequency high temperature sintering; on the temperature control line of this top temperature controlling valu, carry out steady temperature sintering; until reach intermediate frequency high temperature sintering operation full time 240min (± 20min), shielding gas argon flow amount>=2m in intermediate frequency high-temperature sintering process ³/ h; When intermediate frequency high-sintering process processing operation reached after whole intermediate frequency high temperature sintering activity durations of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature; When temperature drops to 380 ℃ in stove, again close immediately fire door, ventilation, energising, start the shaping base substrate in stove to carry out annealing treating process processing operation; The running technology parameter of annealing treating process processing operation is: anneal starting temperature is 380 ℃, with the temperature rise rate continuous warming of 15 ℃/min, after 930 ℃ ﹙ ± 5 ℃ ﹚, stops heating up; In this temperature line, carry out steady temperature annealing, until complete annealing treating process processing operation full time 90min(± 10 min), shielding gas argon flow amount>=0.8m in anneal process ³/ h; Until annealing process processing operation, reach after the anneal operation full time of design, take power-off, die, open the measures such as fire door, rely on shaping base substrate naturally cooling method in stove to lower the temperature, until drop to after room temperature, take out the powder smelting rareearth super magnetostrictive bar goods of sintering sizing.

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