CN102728838B

CN102728838B - Preparing method of molybdenum-based rare earth oxide powder metallurgical alloy wafer

Info

Publication number: CN102728838B
Application number: CN201110091304.XA
Authority: CN
Inventors: 陈雄平; 陈晨
Original assignee: SIPING BEIWEI METAL TECHNOLOGY RESEARCH DEVELOPMENT Co Ltd
Current assignee: Siping Beiwei Molybdenum Industry Limited Company
Priority date: 2011-04-13
Filing date: 2011-04-13
Publication date: 2015-02-11
Anticipated expiration: 2031-04-13
Also published as: CN102728838A

Abstract

The invention discloses a preparing method of a molybdenum-based rare earth oxide powder metallurgical alloy wafer. The method adopts material blending technology of directly mixing three types of rare earth oxide powder in a high proportion into pure molybdenum powder, and employs characteristics of rare earth elements such as long big linkage grains, anti-sag performance and good creep performance and the characteristic that the rare earth element can exert strong dispersion strengthening effects and wrapping effects after adding and compounding to effectively improve the recrystallization temperature of molybdenum and improve the mechanical physical properties of the molybdenum-based alloy material. The method adopts preparing process procedures such as ultrasonic solid phase homogenizing and blending, low-temperature flexible isostatic pressing forming, step-by-step continuous sintering shaping, stagewise multi-pass rolling, and fine processing and grinding, and mating special technical equipment and execution process technical parameters. The method has the characteristics of advanced technology, complete configuration, reliable operation and low cost, and can prepare a molybdenum-based rare earth oxide powder metallurgical alloy wafer with excellent technical performance and high and fine surface quality.

Description

The preparation method of molybdenum-base rare earth powder metallurgy alloy disk

Technical field

The present invention relates to a kind of non-ferrous alloy material, relate to a kind of preparation method of molybdenum-base rare earth powder metallurgy alloy disk specifically.

Technical background

Mo wafer; because its fusing point is high; still have higher intensity and hardness under the high temperature conditions; still can keep excellent electric conductivity and conductivity of heat; there is fabulous stability; be widely used in the production technical field such as Aero-Space, defence and military, metallurgy, electric power, chemical industry, electronics, machinery; particularly in the high-tech products such as high-power transmitting tube, high-voltage large current IGCT and rectifier, high temperature thermoelectric coupling and protection tube, high-temperature electric resistance furnace heat screen, extraordinary electric light source, it is required basic function material.

Developing of molybdenum in China disk is in study, introduces, with reference on the basis of advanced foreign technology, progressively develops and grow up.Last century early sixties, institution of higher learning and the R&D institutions such as Peking University, Zhongnan Polytechnic Univ, Northeastern University, Beijing Non-Ferrous Metal Research General Academy, Shanghai Steel and Iron Research Institute, successively start to translate and introduce about cognitive work of publicity such as the foreign data of Mo wafer and basic theories, and then in succession carried out again the initiative element tasks such as material behavior research, application conditions analysis, product in laboratory, achieve a series of plentiful and substantial scientific achievement.To last century late nineteen eighties, the early 1990s, more domestic scientific researches, production unit successively successfully develop with powder metallurgy process replace casting method make High-Temperature Mo base again rolling be processed into the innovative technology of Mo wafer, the molybdenum-based rare-earth alloy material developing rare earth doped oxide in metal molybdenum makes the innovative technology of Mo wafer, the manufacturing of molybdenum in China disk goods is entered into fast and improves the raising new stage.

Enter 21st century, China's sustain economic high speed development, scientific and technological level rapid advances promotes, under the promotion that market demand sharp increase and external product pour in, Mo wafer goods industry is in all many-sides such as product development development, fabricating technology research and design, commercialization test construction, application device design productions, be obtained for fast development, major scientific and technological achievement continues to bring out.But take a broad view of China's current Mo wafer industry technology present situation, at least in group material proportioning, homogeneous mixture, blank shaping, special technology equipment etc. four, there is significantly not enough or weakness.

The present invention is by manufacturing the investigation analysis of current state of technology to molybdenum in China disk, for deficiency and the weakness of current existence, start with from Basic Theory Analysis, form in the large crucial core technology link of new material three at group material proportioning, process of preparing, special technology equipment etc. targetedly, research and design goes out multinomial innovative technology measure, form the molybdenum-base rare earth powder metallurgy alloy disk technology of preparing that an advanced person is complete, successfully can manufacture out the molybdenum-base rare earth powder metallurgy alloy disk goods with special excellent properties and high-precision surface quality.

Summary of the invention

The technical problem to be solved in the present invention:

The present invention is directed to molybdenum in China disk goods manufacturing technology exist deficiency and weakness, research and design goes out direct vast scale in pure molybdenum powder and mixes polynary group of material proportion technique of 3 kinds of RE oxide powders targetedly, by taking ultrasonic solid phase homogeneous mixture, low temperature flexibility hydrostatic pressing, successively sinter sizing, the rolloff of classification multi-pass, retrofit such as to make at the advanced preparation method, form the preparation method that can manufacture out high-performance and high accuracy molybdenum-base rare earth powder metallurgy alloy disk that an advanced person is complete, and the technical equipment of configuration, the technical parameter performed.

The technical scheme that technical solution problem of the present invention is taked:

The technical problem to be solved in the present invention, intends taking research and design to go out the complete preparation method that can manufacture out high-performance and high accuracy molybdenum-base rare earth powder metallurgy alloy disk of an advanced person, is solved.

The preparation method of the molybdenum-base rare earth powder metallurgy alloy disk of research and design of the present invention, comprise polynary group of material proportioning, ultrasonic homogeneous mixture, low temperature flexibility hydrostatic pressing, successively sinter sizing, the rolloff of classification multi-pass, retrofit are made, commodity finishing and packing 7 road technology of preparing unit, and the technical equipment of configuration, the technical parameter of execution.

Polynary group of described material proportioning technology of preparing unit, is because metal molybdenum has fusing point high (2620 DEG C), still has higher intensity and hardness under the high temperature conditions, still have excellent electrical and thermal conductivity and good stability.But the recrystallization temperature of metal molybdenum lower (1100 DEG C), after recrystallization, to change equiax crystal into by threadiness granular for molecular organization structure, becomes network, and raise along with the temperature of environment for use, and grainiess is sharply grown up vertically, therefore, metal molybdenum is easy brittle failure after depositing annealing, the major defects such as the mechanical and physical performances such as tension, surrender, extension are poor, saw lumber forming difficulty, and the molecular structure of rare earth element is the chain crystal grain of growing up arranged vertically, it is the long brilliant chain bridging arrangement state of dovetail shaped after recrystallization, still there is stronger sagging resistance and good creep properties under the high temperature conditions, can increase the crystal grain of metal molybdenum after adding chemical combination and there is stronger inhibitory action, the recrystallization temperature of metal molybdenum can be improved, thus the mechanical and physical performance of metal molybdenum can be improved, simultaneously, rare earth element all has stronger dispersion-strengthened action again, film can be formed at the grain surface of metal molybdenum after adding chemical combination, play " embedding effect ", gas phase water and oxide can be stoped to deposit at metal molybdenum grain surface, form dispersoid particle, and by dispersoid particle and metal molybdenum molecular network lattice structure generation dislocation effect, thus increase the crystal grain specific area of metal molybdenum, crystal grain thinning granularity, inhibiting grain growth, delay recrystallization tendency, improve the recrystallization temperature of metal molybdenum, improve the mechanical and physical performance of molybdenum-based rare-earth alloy Material texture and shape manufacturability.

The proportioning share of the various batching component of molybdenum-base rare earth powder metallurgy alloy disk: batch to manufacture molybdenum-base rare earth powder metallurgy alloy disk goods gross weight for radix, the proportioning share of various batching component by weight: pure molybdenum powder M ₀93.0 ~ 95.0 parts; Lanthana La ₂o ₃2.2 ~ 2.5 parts; Cerium oxide Ce ₂o ₃1.6 ~ 2.0 parts; Neodymia NdO ₂1.2 ~ 1.5 parts.

Batching component granularity: the powder size of various batching component all≤4 μm.

Batching component purity: the purity of various batching component all >=99.9%; Total impurities adds up to all≤500 μ g/g.

The foundation of polynary group of material proportion technique of research and design of the present invention has: the thermal coefficient of expansion of choice for use 3 kinds of rare earth elements is all very close with metal molybdenum, can keep the non-deformability with metal molybdenum parent basic synchronization under high temperature operating conditions.3 kinds of rare earth elements of choice for use, have higher fusing point and boiling point, La has 2300/4200 DEG C, and Ce has 2272/4050 DEG C, and Nd has 2715/4840 DEG C; Under high temperature (≤1800 DEG C) condition of work can not with metal molybdenum parent phased soln, the excellent specific property of metal molybdenum parent can be maintained preferably.3 kinds of rare earth elements of choice for use, not only have the total good sagging resistance of rare earth element and creep properties, and can have different deep drawing qualities and high plasticity again separately, have good resistance to cold brittleness and non-oxidizability; Can play a significant role to improving molybdenum base material material, particularly mechanical and physical performance and processing serviceability after adding chemical combination.Selection is determined to mix 3 kinds of rare earth oxides with larger proportion simultaneously, makes it mutually support, can fully represent respective characteristic again, more can give full play of the dispersion-strengthened action of rare earth element to metal molybdenum.

Described ultrasonic homogeneous mixture technology of preparing unit, is because ultrasonic wave has extremely strong penetration capacity, in solid medium, also has fabulous conductibility; Ultrasonic wave conducts in solid medium, can cause medium particulate and enter vibrational state, produces and transmits powerful energy, impels medium particulate constantly to carry out displacement movement to antinode or node, forms displacement effect; Although shift length is little, the acceleration be directly proportional to ultrasonic frequency vibratory square is very big, even can exceed several ten thousand times of acceleration of gravity; So huge acceleration energy, is enough to cause that medium particulate strong collision occurs, breaks, the change of mobile isostructuralism.Coordinate simultaneously and adopt mechanical atomization jet agitation mixed technology, the metal dust of each group of material component is injected in the ultrasonic homogeneous blending machine of metal dust with dust cloud state by continuous spraying while of mixed ratio; By the high speed rotary motion of dispersed with stirring device, make to be arranged in dispersed with stirring web obtains high linear velocity and cutting shock metal dust particulate high-frequency along upper hock, thus produce the extremely strong dynamic power such as high speed shear, centrifugal extruding of metal dust particulate; This extremely strong dynamic potential energy, then match with the displacement effect that power ultrasonic produces, be enough to increase quickening metal dust particulate and break, move, collide isostructuralism change.Power ultrasonic and mechanical mixture combine this constructive variations that powder particle is produced, and be enough to the refinement to each batching component metal dust particulate, dispersion, homogeneous play a great role, also effectively can destroy the distinctive reunion adhesion energy of powder particle; Using ultrasound solid phase homogeneous mixed technology, the operation of refinement homogeneous dispersion is implemented to each batching component in solid powder, just can refinement respectively to prepare burden the crystallite size of component, strengthen the homogeneous dispersion degree of each batching component, suppress the growth conditions of thick fragility crystal grain in each batching component, thus improve molybdenum base material material to lay a good foundation condition for improving.

Ultrasonic homogeneous mixture technology of preparing unit, is completed by the ultrasonic homogeneous blending machine of metal dust of original creation design.

The ultrasonic homogeneous blending machine of metal dust, closed circular cone pot structure of container is helped in global design, is made up of, realizes quick opening and closing of fault fixed operation by mounting flange mounting bracket, taper blending tank tank body, blending tank cover; On blending tank cover, be mounted with the operation parts such as 6 metal dust atomization chargers, dispersed with stirring device, safety exhaust; On blending tank tank body, be mounted with vacuum air pump, total terminal box, hydrogen gas injection pump, discharging opening; On the outer wall of blending tank tank body, fix 3 groups of board-like ultrasonic transducers along tank body circumference with a hexagonal angle point position installation, be connected with automaton by total terminal box, bundle conductor.

Board-like ultrasonic transducer, the ultrasonic electric energy that supersonic generator produces can be converted to the high-frequency mechanical vibration ripple with suitable power energy, penetrate blending tank tank skin to conduct in the pink mist metal dust in blending tank, metal dust particulate is made to produce dither, form displacement effect, produce and transmit huge energy.

Vacuum air pump and hydrogen gas injection pump, be fixed on the upper and lower of blending tank tank body respectively.Because rare earth element all has 4f electronic structure; and electronegativity is little; very easily be corroded; particularly high-purity simple substance pulverulence is very responsive to the oxygen in air; for ensureing that rare earth metal powder is being uniformly mixed the purity in operation process; take to vacuum environment filling can the hydrogen of preferential and oxygen chemical combination as safeguard measure, vacuum suction vacuum: 10 × 10 ^-3pa, hydrogen gas injection rate: 0.12m ³/ m ³.

Metal dust atomization charger, is made up of metal dust holding vessel, high-pressure spray pump, powder jet.6 metal dust atomization chargers of design configurations, are fixed on blending tank cover with a point position, concentric circles 60 ° of angles; Wherein 3 load the pure molybdenum powder of equivalent, all the other 3 are respectively charged into other 3 kinds of RE oxide powders, 4 kinds of metal dusts are alternate position distribution, 4 kinds of metal dusts of group material component can be injected in blending tank by mixed ratio continuous spraying with dust cloud state and enter solid phase dispersion homogeneous simultaneously and stir mixture operation.

Dispersed with stirring device, is fixed on blending tank cover center.Select frequency control motor as driving power source, according to the mixture needs of different phase, the adjustment of different rotating speeds change can be made; The employing of dispersed with stirring device is mounted with 2 groups and goes to upper and lower rebuilding on shaft, and each group has 2 hock type dispersed with stirring dishes oppositely installed, the edge of each dispersion impeller be mounted with the structural arrangement form of some hocks.When carrying out dispersed with stirring operation, due to the High Rotation Speed of dispersed with stirring device and the effect of 2 groups of reverse hock type dispersion impellers, in the card of hock type dispersion impeller, all can produce one extremely strong axial attraction separately, pink mist metal dust is sucked from the axial relative direction of card simultaneously fast, flow out to surrounding fast from the centre of 2 groups of dispersion impeller dish back ofs the body again, after encountering blending tank tank skin, respectively to upper, lower both direction flowing, thus driven the whole pink mist metal dusts in blending tank to form the two-way route that stirs continuously to flow fast, eliminate homogeneous dispersion, be uniformly mixed blind area or dead angle that operation may exist.Simultaneously, by the high speed rotary motion of dispersed with stirring device, make design arrangement at some hocks of dispersed with stirring dish periphery, the high-frequency of high linear velocity and the vaporific metal dust of cutting shock can be obtained, thus produce dynamic powers such as the extremely strong high speed shear of metal dust particulate and centrifugal extruding.

Ultrasonic homogeneous mixture technology of preparing unit, it is the elemental metals powder manufacturing various batching constituent element needed for molybdenum-base rare earth powder metallurgy alloy disk, in the ultrasonic homogeneous blending machine of metal dust of configuration, by power ultrasonic vibration displacement, atomized spray, homogeneous dispersion, the engineering means such as to be uniformly mixed, solid phase homogeneous mixture becomes constituent element to be evenly distributed, the molybdenum-based rare-earth alloy powder technology operation process of loose particles specification.

Ultrasonic homogeneous mixture technology of preparing unit, preparation technology's operation technique process is:

---according to the technical requirement of group material proportioning, with batch molybdenum-base rare earth powder metallurgy alloy disk goods gross weight of producing for radix, by the filling rate of metal powder ultrasonic homogeneous blending machine dischargeable capacity 58%, accurately calculate the concrete weight that various batching component elemental metals powder feeds intake.

---according to result of calculation, by the electronic-weighing meter of configuration, after difference Weighing is carried out to various batching component elemental metals powder, be respectively charged into and be arranged in metal dust atomization charger corresponding on the ultrasonic homogeneous blending machine of metal dust.

---start vacuum air pump, extract the air in blending tank out; Vacuum reaches 12 × 10 ^-3during Pa, close vavuum pump.

---start hydrogen gas injection pump immediately, injecting gas hydrogen in blending tank; Gas injection rate reaches 0.12m ³/ m ³time, close gas injection pump.

---start 6 metal dust atomization chargers immediately simultaneously; Under the effect of high-pressure spray pump, the elemental metals powder of 4 kinds of batching constituent elements by powder jet, inject in blending tank by mixed ratio with continuous spraying while of pink mist; Whole material spray time controling completes in 18 ~ 20min.

---meanwhile start dispersed with stirring device, with the rotating speed High Rotation Speed of 1200r/min, drive to spray and flow fast with the two-way route that stirs continuously into all metal powder granulates of the pink mist in blending tank, and the shock accepting to be arranged on the dynamic power such as high-speed cutting, centrifugal extruding of dispersed with stirring dish periphery hock cuts and dispersion is uniformly mixed operation, the dither formed with power ultrasonic, displacement effect match, and complete the homogeneous dispersion to multiple elemental metals powder, be uniformly mixed operation.

---meanwhile start the supersonic generator in automaton, ultrasonic electric energy is coupled on board-like ultrasonic transducer, is converted to by board-like ultrasonic transducer and there is 42KH _zfrequency and 4.2w/cm ²the power ultrasonic of the sound intensity, to spraying into all metal powder granulates conduct radiation of the pink mist in blending tank, cause dither and displacement effect, stir with mechanical dispersion the dynamic potential energy formed to match, make metal powder granulates produce displacement, collide, isostructuralism of breaking change, just can give play to powerful crystal grain thinning granularity, strengthen the effect of homogeneous dispersion degree.The Ultrasonic Radiation time closes supersonic generator after reaching 25 ~ 28min.

---after Ultrasonic Radiation stops, dispersed with stirring device works on 3 ~ 5min; After cut out dispersed with stirring device stops operation 10min, open discharging opening, take out the molybdenum-based rare-earth alloy powder that homogeneous mixture is made.

Described low temperature flexibility hydrostatic pressing technology of preparing unit, because cryogenic forming is the advanced and sophisticated technology of Powder Metallurgy Industry, by having the shaping dies of low-temperature heat function, when molybdenum-based rare-earth alloy powder is heated to 60 ~ 70 DEG C, larger activation energy can be formed in alloy powder.This activation energy, can improve the mechanical interlocking between alloy powder particle and surface atom attraction, increases the intensity of shaping base substrate; The mobility of alloy powder particle can be improved, increase density and the homogeneous degree of shaping base substrate; The oxygen reduction speed of rare earth oxide can also be improved, avoid or reduce in shaping base substrate occurring the tissue defects such as crackle, bubble, shrinkage porosite.The power resources be shaped due to alloy powder densification rely on pressure fine and close, after requiring that this pressure dynamics must be able to make alloy powder particle all produce brittle fracture, could form new body again; But if alloy powder applied pressure is uneven, or insufficient pressure, time are inadequate, only will there occurs elastic deformation by some alloy powder particle, also plastic deformation not occur, do not produce brittle fracture; If now pressure relief, just may there is bounce-back or restore to the original state in these powder particles that elastic deformation only occurs, therefore neomorph inside just there will be expansion, shrinkage porosite, or produce underbead crack, leaves major quality hidden danger.Therefore, must guarantee that the isostasy of exerting pressure is lastingly powerful, make alloy powder particle all produce brittle fracture, qualified neomorph is formed in densification.

Low temperature flexibility hydrostatic pressing technology of preparing unit, the heating shaping dies designed by original creation and horizontal bidirectional flexible hydraulic harder complete.

Heating shaping dies, by left and right movable pressing board, pressing plate loose slot, cover plate, base, powder loads die cavity and electrical heating elements forms.Heating shaping dies is fixed on hydraulic pressure harder workbench, and the right movable pressing board of mould is connected with right oil cylinder pressure head, and the left movable pressing board of mould is connected with left oil cylinder pressure head; Forming dextrad pressure densification operation unit by right oil cylinder pressure head, right oil cylinder, right cylinder bracket and right oil cylinder oil pipe, by there being cylinder bracket to be fixed on hydraulic pressure harder workbench, being connected with hydraulic control system case by right oil cylinder oil pipe; Form left-hand pressure densification operation unit by left oil cylinder pressure head, left oil cylinder, left cylinder bracket and left oil cylinder oil pipe, be fixed on hydraulic pressure harder workbench by left cylinder bracket, be connected with hydraulic control system case by left oil cylinder oil pipe.Hydraulic control system case is fixed on by hydraulic pressure harder lathe bed, and the hydraulic work system parts such as motor, hydraulic oil container, gear oil pump, control valve, distributing valve, overflow valve, safety valve, Monitoring and Controlling instrument, maneuvering and control panel are equipped with in inside.

Low temperature flexibility hydrostatic pressing technology of preparing unit, that molybdenum-based rare-earth alloy powder the project slash such as to be exerted pressure by heating shaping mold heated, bidirectional flexible isostatic pressed, pressure densification become to have definite shape size, pressurized general equilibrium, Density Distribution evenly, molybdenum-base rare earth powder metallurgy alloy blank technological processes that structural strength is larger.

Low temperature flexibility hydrostatic pressing technology of preparing unit, preparation technology's operation technique process is:

---concrete needs such as density, net weight, shape, size etc. required by molybdenum-base rare earth powder metallurgy alloy disk goods, take into full account the factor such as consumption, scaling loss, porosity, sintering shrinkage in hydrostatic pressing and sintering type-approval process, accurately calculate the densification of this batch press and be formed in the concrete weight of molybdenum-based rare-earth alloy powder that powder loads die cavity planted agent filling.

---according to result of calculation, by the electronic-weighing meter of configuration, after Weighing is carried out to molybdenum-based rare-earth alloy powder, load powder and load jolt ramming in die cavity.

---start the electric heating device of heating shaping dies, the molybdenum-based rare-earth alloy powder be contained in powder filling die cavity is heated to 60 ~ 70 DEG C.

---start horizontal bidirectional flexible hydraulic harder, the bidirectional flexible isostatic pressed that has of hydraulic system is relied on to exert pressure function, make left and right two oil cylinders can with the powerful flexible working pressure of the stable and uniform operating rate of 8mm/min and 300MPa, from left and right both direction with equivalent pressure and speed, stable and uniform ground promotes the left and right movable pressing board of heating shaping dies, applies powerful pliable pressure to the molybdenum-based rare-earth alloy powder of existing uniform temperature; The fixed form of heating shaping dies surrounding, the reaction force equal with this pressure is formed under impressed pressure effect, exert pressure to molybdenum-based rare-earth alloy powder surrounding simultaneously, make the powder molybdenum-based rare-earth alloy powder loaded in die cavity receive simultaneously each to brute force exert pressure, and make each to pressurized general equilibrium.

---the left and right movable pressing board of heating shaping dies, stops mobile when being advanced to the gear be provided with, although now left and right oil cylinder can not continue to advance, still remain the operational pressure of 300MPa, and continue to be applied on molybdenum-based rare-earth alloy powder; After horizontal bidirectional flexible hydraulic harder keeps voltage stabilizing 40min under this operational pressure, take to reduce pressure gradually stage by stage unloading pressure means: decompression rate all-the-time stable controls at 6MPa/min; First time unloads and is pressed onto 270MPa, voltage stabilizing 10min; Second time is unloaded and is pressed onto 210MPa, then voltage stabilizing 5min; Third time unloads and is pressed onto 120Mpa, then voltage stabilizing 5min; Press the whole pressure of decompression rate removal of 6MPa/min for 4th time.

---demoulding, takes out the molybdenum-base rare earth powder metallurgy alloy blank that pressure densification is shaped.

Described successively sintering sizing technology of preparing unit, by taking successively to carry out the PM technique means such as low-temperature bake, middle temperature presintering, the sizing of intermediate frequency high temperature sintering continuously in hydrogen atmosphere, after making the great variety such as molybdenum-base rare earth powder metallurgy alloy blank shrinks densification, intensity increases, the stable raising of physical and chemical performance, be prepared into surface without sizing dirtyization, the inner molybdenum-base rare earth powder metallurgy alloy rolloff blank technological processes be evenly distributed without hierarchical crack, tissue density.

Successively sintering sizing technology of preparing unit, is configured with the special technology equipments such as hydrogen atmosphere low-temperature bake stove, hydrogen atmosphere intermediate sintering temperature stove, hydrogen atmosphere intermediate frequency high temperature sintering furnace.

Successively sintering sizing technology of preparing unit, preparation technology's operation technique process is:

First low-temperature bake technical operation is carried out:

---molybdenum-base rare earth powder metallurgy alloy blank is put in hydrogen atmosphere low-temperature bake stove, lower temperature is used to carry out low-temperature bake, bond strength between the molybdenum-based rare-earth alloy particle in blank can be made to increase, and on link surface, gravitational force between atoms increases, and makes to occur between alloying pellet to attract bonding fixing; Can eliminate the partial elastic internal stress dissolving blank when pressure densification is shaped, most of gas and the moisture content of blank absorption are got rid of in volatilization simultaneously.The heating rate stability contorting of low-temperature bake is at 10 DEG C/min (± 2 DEG C), and the highest baking temperature controls at 480 DEG C (± 5 DEG C), and whole baking time controls at 100min (± 10min); In bake process, hydrogen flowing quantity stability contorting is at>=0.8m ³/ h.Low-temperature bake reaches power-off after baking time, by Temperature fall method cooling in stove; When in-furnace temperature is down to 120 DEG C, baking blank rotary is delivered in intermediate sintering temperature stove carry out intermediate sintering temperature technical operation immediately.

Next carries out middle temperature presintering technical operation:

---the baking blank with more than 120 DEG C temperature is put into and is preheating in the hydrogen atmosphere intermediate sintering temperature stove of equal temperature, sufficient temp is used to carry out intermediate sintering temperature, make to produce larger activation energy in blank, the atom amplitude of molybdenum-based rare-earth alloy particle is allowed to strengthen, abundant atom is made to enter in atomic attraction sphere of action, atom is impelled to pass through evaporation, diffusion, flowing, the multiple migration forms such as cohesion, crystal grain boundary is formed between molybdenum-based rare-earth alloy particle, and progressively move to granule interior, thus make the intergranular Distance Shortened of molybdenum-based rare-earth alloy, porosity reduces, density increases, finally make the volume contraction of molybdenum-base rare earth powder metallurgy alloy blank, the oxide of molybdenum-based rare-earth alloy particle surface can be made to be completely reduced, gas, the moisture content of blank absorption are excluded entirely volatilization simultaneously, and the internal stress that blank is formed in pressure densification is shaped obtains thoroughly eliminating dissolving.The heating rate stability contorting of intermediate sintering temperature is at 15 DEG C/min (± 2 DEG C), most senior middle school temperature sintering temperature controls at 980 DEG C (± 5 DEG C), whole intermediate sintering temperature time controling is within 150min (± 10min), and in sintering process, hydrogen flowing quantity stability contorting is at>=1.5m ³/ h.Intermediate sintering temperature reaches power-off after sintering time, by Temperature fall method cooling in stove; When in-furnace temperature is down to 250 DEG C, intermediate sintering temperature blank rotary is delivered in intermediate frequency high temperature sintering furnace carry out the operation of high temperature sintering shaping technology immediately.

Finally carry out the operation of high temperature sintering shaping technology:

---the intermediate sintering temperature blank with more than 250 DEG C temperature is put into and is preheating in the hydrogen atmosphere intermediate frequency high temperature sintering furnace of equal temperature, higher temperature is used to carry out the high temperature sintering sizing of long period, blank atoms permeating and flowing are fully carried out, blank hole and size are fully reduced, and it is stable that the established good mechanical physical property of blank obtains best reservation.The heating rate of high temperature sintering sizing is divided into 3 stages: from 250 DEG C of temperature, with the heating rate continuous warming 20min of 15 DEG C/min (± 2 DEG C), make furnace temperature reach 550 DEG C, steady temperature 10min; Again with the programming rate continuous warming 30min of 10 DEG C/min (± 2 DEG C), furnace temperature is made to reach 850 DEG C, steady temperature 35min; Again with the highest controlling value 1225 DEG C (± 5 DEG C) of the programming rate continuous warming of 15 DEG C/min (± 2 DEG C) to intermediate frequency high temperature sintering temperature; In this temperature line, steady temperature sintering 120min, whole sintering times that high temperature Median frequency sintering is shaped control at 240min (± 10min).In intermediate frequency high temperature sintering type-approval process, hydrogen flowing quantity stability contorting is at>=2m ³/ h.Intermediate frequency high temperature sintering reaches power-off after sintering time, by Temperature fall method cooling in stove; After in-furnace temperature is down to normal temperature, take out the molybdenum-base rare earth powder metallurgy alloy rolloff blank made.

Described classification multi-pass rolloff technology of preparing unit, by taking the classification multi-pass rolloff technological means such as horizontal cogging breaking down, longitudinal roughing, precision cold-rolled in general roll off plant equipment, make molybdenum-base rare earth powder metallurgy alloy rolloff blank can complete to goods Forms Transformation in all many-sides such as interior tissue, geometry, mechanical and physical performances, be prepared into and be convenient to the molybdenum-base rare earth powder metallurgy sheet alloy technological processes that orienting articles is processed in meticulous in-depth.

Classification multi-pass rolloff technology of preparing unit, is configured with the current techique equipments such as hydrogen atmosphere heating furnace, hydrogen atmosphere annealing furnace, four roller reversible hot milling rolls, the reversible precise cold milling train of four rollers, plate shearing machine.

Classification multi-pass rolloff technology of preparing unit, preparation technology's operation technique process is:

First multi-pass horizontal cogging breaking down technical operation is carried out:

---molybdenum-base rare earth powder metallurgy alloy rolloff blank is put in hydrogen atmosphere heating furnace, carries out the first fire heating; Heating-up temperature 1200 ~ 1300 DEG C, heat time 80 ~ 90min, hydrogen flowing quantity>=0.8m ³/ h.After completing heating operation, immediately rolloff blank is laterally put in four roller reversible hot milling rolls, carry out continuous 3 passage lateral shuttle cogging breaking down technical operations; Hot mill rolling power >=400t, roll specification Φ 180 × 400mm, mill speed≤30m/min, on average every time working modulus >=15%.

---after completing the first fiery heating rolling, immediately rolloff blank is put in hydrogen atmosphere heating furnace again, carry out the second fire heating; Heating-up temperature 1100 ~ 1200 DEG C, heat time 40 ~ 50min, hydrogen flowing quantity>=0.8m ³/ h.After completing heating operation, immediately rolloff blank is laterally put in four roller reversible hot milling rolls again, still use≤the mill speed of 30m/min, then carry out continuously taking turns 3 passage lateral shuttle cogging breaking down operations; Every time working modulus >=20% average.

---after completing the 2nd fiery heating rolling, immediately rolloff blank is put in hydrogen atmosphere annealing furnace, carry out the process of annealing heat retaining operation; Annealing temperature 850 ~ 870 DEG C, annealing high temperature hold time 30 ~ 40min, hydrogen flowing quantity>=0.5m ³/ h.Reach annealing temperature retention time after power-off, stop hydrogen supply; Rolloff blank takes out after Temperature fall cooling in hydrogen atmosphere annealing furnace.

Multi-pass horizontal cogging breaking down operation is carried out in design arrangement, all selects cross rolling in the rolling direction, can reduce the anisotropy on blank structure and properties, improve blank horizontal plastic property; Select to adopt higher heating-up temperature and larger pass reduction, blank can be made to obtain larger draught pressure, ensure that blank atom enters metallic bond gravisphere, make the raising of blank intercrystalline bond strength, density increase, can avoid occurring the mass defect such as interlayer, crackle; Select to adopt higher anneal temperature and longer annealing temperature retention time, blank can be made to obtain more processing texture structure, avoid the recrystallization of metal molybdenum to occur, effectively can eliminate the internal stress of blank, improve blank rolloff become sheet material after room temperature mechanical physical property.

Next carries out the longitudinal roughing technical operation of multi-pass:

---the rolloff blank through cogging breaking down is put in hydrogen atmosphere heating furnace, carries out the first fire heating; Heating-up temperature 950 ~ 1050 DEG C, heat time 70 ~ 80min, hydrogen flowing quantity>=0.8m ³/ h.After completing heating operation, immediately rolloff blank is longitudinally put on four roller reversibly hot milling trains, carry out continuous 3 passages and longitudinally come and go roughing operation; Hot mill rolling power >=400t, roll specification Φ 180 × 400mm, mill speed≤45m/min, on average every time working modulus≤12%.

---after completing the first fiery heating rolling, immediately rolloff blank is put in hydrogen atmosphere heating furnace again, carry out the 2nd fire heating; Heating-up temperature 900 ~ 1000 DEG C, heat time 40 ~ 50min, hydrogen flowing quantity>=0.8m ³/ h.After completing heating operation, immediately rolloff blank is put on four roller reversible hot milling rolls again, still use≤the mill speed of 45m/min, then carry out taking turns 3 passages continuously and longitudinally come and go roughing operation, on average every time working modulus≤10%, be rolled into rolloff plate.

---after completing the 2nd fiery heating rolling, immediately rolloff plate is put in hydrogen atmosphere annealing furnace, carry out the process of annealing heat retaining operation; Annealing temperature 850 ~ 870 DEG C, annealing high temperature hold time 50 ~ 60min, hydrogen flowing quantity>=0.5m ³/ h.Reach annealing temperature retention time after power-off, stop hydrogen supply; Rolloff plate takes out after Temperature fall cooling in hydrogen atmosphere annealing furnace.

---by completing longitudinal roughing and the cooled rolloff plate of annealing, deliver on plate shearing machine, at the beginning of carrying out, the correction of the flank shape of step cutting edge, excise limit more than irregular calendering, can reduce precision cold-rolled power consumption, the tailing reclaiming molybdenum-based rare-earth alloy rolloff plate in time utilizes.

Design arranges the longitudinal roughing operation of multi-pass, all select longitudinal rolling in the rolling direction, can cooperatively interact with the horizontal breaking down of cogging, form a kind of commutation tandem rolling technical method, slab interior tissue is distributed to reasonable direction, anisotropy is obviously reduced, and the plate of rolling can be made two-wayly can to obtain unified better technical performance longitudinal and transverse; Select to adopt lower heating-up temperature and less pass reduction, the geometry of rolloff plate can be finalized the design almost, acquired excellent mechanical physical property obtains retaining preferably stablizing.

Finally carry out multi-pass precision cold-rolled technical operation:

---the rolloff panel surface will carrying out precision cold-rolled is thoroughly cleared up, avoids the hard such as burr, the decortication foreign material adhered to that panel surface is caused to impression, draws the mass defects such as mark.After completing prune job, smear thin layer cold-rolling lubricant with cotton yarn in panel surface.

---the rolloff plate through removing surface is longitudinally put on the reversible precise cold milling train of four rollers, carries out first time continuous 3 passages longitudinally round precision cold-rolled; Roll-force >=the 400t of precise cold milling train, roll specification Φ 180 × 400mm, mill speed≤60m/min, on average every time working modulus≤5%.

---will the plate after the 1st precision cold-rolled be completed, carry out again surface thoroughly cleaning; Again smear cold-rolling lubricant with cotton yarn in panel surface.

---the plate through the 2nd subsurface cleaning is longitudinally put on the reversible precise cold milling train of four rollers again, still with the mill speed of≤60m/min, then carries out 3 passages continuously and longitudinally come and go precision cold-rolled, on average every time working modulus≤2%; Molybdenum-base rare earth powder metallurgy sheet alloy is made in final rolloff, and reaches the gauge tolerance standard that technical papers specifies.

Technology of preparing unit is made in described retrofit: be by taking the retrofits such as Blanking Shaping, elementary grinding, precise finiss to make technological means on special-purpose machinery process equipment, manufacturing out the technological processes of molybdenum-base rare earth powder metallurgy alloy disk goods.

Technology of preparing unit is made in retrofit, is configured with the current techique equipments such as hydraulic plate shears, hydraulic press, disk grinder, disc type precision lapping machine.

Technology of preparing unit is made in retrofit, and preparation technology's operation technique process is:

---sheet material is put on hydraulic plate shears, by the molybdenum-base rare earth powder metallurgy alloy disk product specifications size using user's requirement, use pliable pressure to be cut into bar shaped plate; Configuration hydraulic plate shears cut out thickness 0.8 ~ 4.0mm, cut out length >=1000mm.

---bar shaped plate is put on hydraulic press, by disk hydraulic pressure blanking die, by the specification tolerance of molybdenum-base rare earth powder metallurgy alloy disk goods, uses the circular sheet stock of pliable pressure stamping-out; Stamping-out pressure >=the 100t of hydraulic press, rushes circular diameter Φ 25 ~ 110mm, punching circle thickness 0.8 ~ 4.0mm.

---circular sheet stock is put on disk grinder and carry out elementary attrition process; Use common cooling fluid during elementary grinding, allowance 0,06 ~ 0.08mm, lap speed selects 800 ~ 1000r/min.

---the circular sheet stock through elementary grinding is put on disc type precision lapping machine, finally makes fine gtinding processing; Fine gtinding adds man-hour, grinding agent choice for use W20 schmigel+20 ^#machine oil (proportioning 1:15 ~ 20), lap speed selects 1500 ~ 2000r/min.

Described commodity finishing and packing technology of preparing unit is the technical standard requirement of dispatching from the factory according to molybdenum-base rare earth powder metallurgy alloy disk goods, carries out the commercial treatment such as clean and tidy, cleaning, anticorrosion, mark, anticollision packaging; After completing, pin is treated in warehouse-in keeping.

The advantage that the present invention has and the effect reached:

1, the direct vast scale in pure molybdenum powder of research and design of the present invention mixes polynary group of material proportioning innovative technology of 3 kinds of RE oxide powders, make full use of rare earth element to the distinctive dispersion-strengthened action of metal molybdenum and embedding effect, effectively improve the intensity of molybdenum-based rare-earth alloy Material texture, toughness and plasticity, improve processing serviceability, expand range of application.

2, the ultrasonic solid phase homogeneous mixture innovative technology of research and design of the present invention, make full use of power ultrasonic and can produce high-frequency, high strength, high-energy mechanical oscillation function and displacement effect, match with traditional mechanical atomization jet agitation hybrid technology, the crystallite size of refinement batching group element material effectively, enhance homogeneous dispersion degree, destroy the reunion adhesion energy cleared up powder particle and very easily produced, simplify preparation technology, reduce preparation cost.

3, the low temperature flexibility hydrostatic pressing innovative technology of research and design of the present invention, do not add any bonding agent, lubricant, the low-temperature heat function of shaping dies and the bidirectional flexible isostatic pressed of harder hydraulic system is relied on to exert pressure function, make molybdenum-based rare-earth alloy powder particle in all directions, powerful equalization stable equivalent pressure can be accepted simultaneously, complete and develop to complete brittle fracture from elastic deformation, become the neomorph of pressure densification, solve in the fine and close shaping base substrate of traditional liquid pressure medium and often there is expansion, shrinkage porosite, the major quality potential problems such as crackle, effectively improve the material quality of molybdenum original washing powder smelting rare earth alloy blank, for follow-up saw lumber in-depth processing creates advantage, provide robust techniques quality assurance.

4, the successively continuous sintering sizing innovative technology of research and design of the present invention, by molybdenum-based rare-earth alloy powder after low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering sizing continuous sintering process, shaping base substrate can be made to become, and a kind of volume contraction is closely knit, tissue intensity improves, the stable sintered metal product of mechanical and physical performance, for the same industry provide a kind of can the new technology of reference.

Accompanying drawing explanation

Accompanying drawing 1: molybdenum-base rare earth powder metallurgy alloy disk preparation method technology path schematic diagram.

Accompanying drawing 2: metal dust ultrasonic homogeneous blending machine structural principle schematic diagram.

Accompanying drawing 3: horizontal bidirectional flexible hydraulic harder structural principle schematic diagram.

Detailed description of the invention

As shown in Figure 1, the preparation method of molybdenum-base rare earth powder metallurgy alloy disk of the present invention, comprise polynary group of material proportioning (I), ultrasonic homogeneous mixture (II), low temperature flexibility hydrostatic pressing (III), successively sinter sizing (IV), classification multi-pass rolloff (V), retrofit make (VI), commodity finishing and packing (VII) 7 road technology of preparing unit, and the technical equipment of configuration, the technical parameter of execution.

As shown in Figure 1, polynary group of described material proportioning technology of preparing unit (I), determine the proportioning share of molybdenum-base rare earth powder metallurgy alloy disk various groups of material components, batch to manufacture molybdenum-base rare earth powder metallurgy alloy disk goods gross weight for radix, the proportioning share of various batching component by weight: pure molybdenum powder M ₀93.0 ~ 95.0 parts; Lanthana La ₂o ₃2.2 ~ 2.5 parts; Cerium oxide Ce ₂o ₃1.6 ~ 2.0 parts; Neodymia NdO ₂1.2 ~ 1.5 parts.

As shown in accompanying drawing 1, accompanying drawing 2, described ultrasonic homogeneous mixture technology of preparing unit (II), is completed by the ultrasonic homogeneous blending machine of metal dust of original creation design.The ultrasonic homogeneous blending machine of metal dust, closed circular cone pot structure of container is helped in global design, be made up of mounting bracket (14), taper blending tank tank body (11), blending tank cover (9), realize quick opening and closing of fault fixed operation by mounting flange (10); On blending tank cover (9), be mounted with the operation parts such as 6 metal dust atomization chargers (7), dispersed with stirring device (4), safety exhaust (8); On blending tank tank body (11), be mounted with vacuum air pump (6), total terminal box (3), hydrogen gas injection pump (12), discharging opening (13); On the outer wall of blending tank tank body (11), install and fix 3 groups of board-like ultrasonic transducers (5), be connected with automaton (1) by total terminal box (3), bundle conductor (2).

Board-like ultrasonic transducer (5), along blending tank tank body (11) outer wall with 120.It is fixing that angle divides position to install, and the power ultrasonic with suitable power energy can be conducted in the pink mist metal dust in blending tank to spraying, and makes metal powder granulates produce dither, form displacement effect, produce and transmit huge energy.Metal dust atomization charger (7), is made up of metal dust holding vessel, high-pressure spray pump, powder jet; 6 metal dust atomization chargers (7) of configuration, be fixed on blending tank cover (9) with a point position, concentric circles 60 ° of angles, wherein 3 load the pure molybdenum powder of equivalent, all the other 3 are respectively charged into 3 kinds of RE oxide powders, make 4 kinds of metal dusts be alternate position distribution, 4 kinds of metal dusts of group material component can be injected in blending tank by continuous spraying while of mixed ratio with dust cloud state.Dispersed with stirring device (4), is fixed on blending tank cover (9) center, selects frequency control motor as driving power source, according to the mixture needs of different phase, can make the adjustment of different rotating speeds change, dispersed with stirring device (4) is mounted with 2 groups and goes to upper and lower rebuilding on shaft, and each group has 2 hock type dispersed with stirring dishes oppositely installed, and the periphery of each dispersion impeller is mounted with some hocks, when carrying out dispersed with stirring operation, due to the High Rotation Speed of dispersed with stirring device (4) and the effect of 2 groups of reverse hock type dispersion impellers, the card of each hock type dispersion impeller can produce one extremely strong axial attraction, pink mist metal dust is sucked from the axial relative direction of card simultaneously fast, flow out to surrounding fast from the centre of 2 dispersion impeller dish back ofs the body again, can respectively to upper after encountering blending tank tank skin, lower both direction flowing, thus driven the whole pink mist metal dusts in blending tank to form the two-way route that stirs continuously to flow fast, eliminate homogeneous dispersion, be uniformly mixed blind area or dead angle that operation may exist, simultaneously, by the high speed rotary motion of dispersed with stirring device (4), make design arrangement at some hocks of dispersed with stirring dish periphery, the high-frequency of high linear velocity and cutting shock atomized metal pow der can be obtained, thus produce dynamic powers such as the extremely strong high speed shear of metal dust particulate and centrifugal extruding.

Ultrasonic homogeneous mixture technology of preparing unit (II), the elemental metals powder of various batching component, solid phase homogeneous mixture be prepared into composite distribution evenly, the molybdenum-based rare-earth alloy powder technology operation technique process of loose particles specification is:

---according to result of calculation, by the electronic-weighing meter of configuration, after difference Weighing is carried out to various batching component elemental metals powder, be respectively charged in corresponding metal dust atomization charger (7).

---start vacuum air pump (6), extract the air in blending tank out; Vacuum reaches 12 × 10 ^-3during Pa, close vavuum pump.

---start hydrogen gas injection pump (12) immediately, injecting gas hydrogen in blending tank; Gas injection rate reaches 0.12m ³/ m ³time, close gas injection pump.

---start 6 metal dust atomization chargers (7) immediately simultaneously; Under the effect of high-pressure spray pump, the elemental metals powder of 4 kinds of batching components by powder jet, inject in blending tank by mixed ratio with continuous spraying while of pink mist; Whole material spray time controling completes in 18 ~ 20min.

---meanwhile start dispersed with stirring device (4), with the rotating speed High Rotation Speed of 1200r/min, drive to spray and flow fast with the two-way route that stirs continuously into all pink mist metal powder granulates in blending tank, and the shock accepting to be arranged on the dynamic power such as high-speed cutting, centrifugal extruding of dispersed with stirring dish periphery hock cuts and dispersion is uniformly mixed operation, the dither formed with power ultrasonic, displacement effect match, and complete the homogeneous dispersion to multiple elemental metals powder, be uniformly mixed operation.

---meanwhile, start the supersonic generator in automaton (1), ultrasonic electric energy is coupled on board-like ultrasonic transducer (5), is converted to by board-like ultrasonic transducer (5) and there is 42KH _zfrequency and 4.2w/cm ²the power ultrasonic of the sound intensity, to spraying conduct radiation in all pink mist metal powder granulates in blending tank, cause dither and displacement effect, stir with mechanical dispersion the dynamic potential energy formed to match, make metal powder granulates produce displacement, collide, isostructuralism of breaking change, given play to powerful crystal grain thinning granularity, the effect of strengthening homogeneous dispersion degree.The Ultrasonic Radiation time closes supersonic generator after reaching 25 ~ 28min.

---after Ultrasonic Radiation stops, dispersed with stirring device (4) works on 3 ~ 5min; Disperser to be mixed (4) stops operation after 10min, opens discharging opening (13), takes out the molybdenum-based rare-earth alloy powder that mixture is made.

As shown in accompanying drawing 1, accompanying drawing 3, described low temperature flexibility hydrostatic pressing technology of preparing unit (III), the heating shaping dies designed by original creation and horizontal bidirectional flexible hydraulic harder complete.Heating shaping dies, by right movable pressing board (20), left movable pressing board (25), pressing plate oriented movable groove (19), cover plate (22), base (23), powder loads die cavity (24) and electrical heating elements forms; Heating shaping dies is fixed on harder workbench (29), the right movable pressing board of mould (20) is connected with right oil cylinder pressure head (21), and the left movable pressing board of mould (25) is connected with left oil cylinder pressure head (26); Dextrad pressure densification operation unit is formed by right oil cylinder pressure head (21), right oil cylinder (18), right cylinder bracket (17) and right oil cylinder oil pipe (16), be fixed on harder lathe bed (15) by right cylinder bracket (17), be connected with hydraulic control system case (31) by right oil cylinder oil pipe (16); Left-hand pressure densification operation unit is formed by left oil cylinder pressure head (26), left oil cylinder (28), left cylinder bracket (27) and left oil cylinder oil pipe (30), be fixed on harder lathe bed (15) by left cylinder bracket (27), be connected with hydraulic control system case (31) by left oil cylinder oil pipe (30).It is other that hydraulic control system case (31) is fixed on harder lathe bed (15), and the hydraulic work system parts such as motor, hydraulic oil container, gear oil pump, control valve, distributing valve, overflow valve, safety valve, Monitoring and Controlling instrument, maneuvering and control panel are equipped with in inside.

Low temperature flexibility hydrostatic pressing technology of preparing unit (III), the densification of molybdenum-based rare-earth alloy powder pressure be prepared into have definite shape size, pressurized general equilibrium, Density Distribution evenly, molybdenum-base rare earth powder metallurgy alloy blank process operation technical process that structural strength is larger is:

---concrete needs such as density, net weight, shape, size etc. required by molybdenum-base rare earth powder metallurgy alloy disk goods, take into full account the factor such as consumption, scaling loss, porosity, sintering shrinkage in hydrostatic pressing and sintering type-approval process, accurately calculate the densification of this batch press and be formed in the concrete weight of molybdenum-based rare-earth alloy powder that powder loads die cavity (24) planted agent filling.

---according to result of calculation, by the electronic-weighing meter of configuration, after Weighing is carried out to molybdenum-based rare-earth alloy powder, load powder and load die cavity (24) interior jolt ramming.

---start the electric heating device of heating shaping dies, the molybdenum-based rare-earth alloy powder be contained in powder filling die cavity (24) is heated to 60 ~ 70 DEG C.

---start horizontal bidirectional flexible hydraulic harder, the bidirectional flexible isostatic pressed that has of hydraulic system is relied on to exert pressure function, make left and right two oil cylinders (28), (18) can with the powerful flexible working pressure of the stable and uniform operating rate of 8mm/min and 300MPa, from left and right both direction with equivalent pressure and speed, stable and uniform ground promotes left and right movable pressing board (25), (20) of heating shaping dies, applies powerful pliable pressure to the molybdenum-based rare-earth alloy powder of existing uniform temperature; The fixed form of heating shaping dies surrounding, the reaction force equal with this pressure is formed under impressed pressure effect, exert pressure to molybdenum-based rare-earth alloy powder surrounding simultaneously, make the powder molybdenum-based rare-earth alloy powder loaded in die cavity (24) receive simultaneously each to brute force exert pressure, and make each to pressurized general equilibrium.

---stop mobile when the left and right movable pressing board (25) of heating shaping dies, (20) are advanced to the gear be provided with, now left and right oil cylinder (28), (18) are although can not continue to advance, but still remain the operational pressure of 300MPa, and continue to be applied on molybdenum-based rare-earth alloy powder; After horizontal bidirectional flexible hydraulic harder keeps voltage stabilizing 40min under this operational pressure, take stage by stage unloading pressure means gradually: decompression rate all-the-time stable controls at 6MPa/min; First time unloads and is pressed onto 270MPa, voltage stabilizing 10min; Second time is unloaded and is pressed onto 2i0MPa, then voltage stabilizing 5min; Third time unloads and is pressed onto 120Mpa, then voltage stabilizing 5min; Press the whole pressure of decompression rate removal of 6MPa/min for 4th time.

As shown in Figure 1, described successively sintering sizing technology of preparing unit (IV), comprise low-temperature bake, middle temperature presintering, continuous three sintering works of intermediate frequency high temperature sintering sizing, can make the great variety such as molybdenum-base rare earth powder metallurgy alloy blank shrinks densification, intensity increases, stable raisings of physical and chemical performance, being prepared into the molybdenum-base rare earth powder metallurgy alloy rolloff blank process operation technical process that surface is evenly distributed without hierarchical crack, tissue density without sizing dirtyization, inside is:

First low-temperature bake technical operation is carried out:

---molybdenum-base rare earth powder metallurgy alloy blank is put in hydrogen atmosphere low-temperature bake stove, lower temperature is used to carry out low-temperature bake, bond strength between the molybdenum-based rare-earth alloy particle in blank can be made to increase, and on link surface, gravitational force between atoms increases, and makes to occur between alloying pellet to attract bonding fixing; Can eliminate the partial elastic internal stress dissolving blank when pressure densification is shaped, most of gas and the moisture content of blank absorption are got rid of in volatilization simultaneously.The heating rate stability contorting of low-temperature bake is at 10 DEG C/min (± 2 DEG C), the highest baking temperature controls at 480 DEG C (± 5 DEG C), whole baking time controls at 100min (± 10min), and in bake process, hydrogen flowing quantity stability contorting is at>=0.8m ³/ h.Low-temperature bake reaches power-off after baking time, by Temperature fall method cooling in stove; When in-furnace temperature is down to 120 DEG C, baking blank rotary is delivered in intermediate sintering temperature stove carry out intermediate sintering temperature technical operation immediately.

Next carries out middle temperature presintering technical operation:

As shown in Figure 1, described classification multi-pass rolloff technology of preparing unit (V), comprise horizontal cogging breaking down, longitudinal roughing, precision cold-rolled three grades of rolloff operations, molybdenum-based rare-earth alloy rolloff blank can be made all to complete to goods Forms Transformation in all many-sides such as interior tissue, geometry, mechanical and physical performances, be prepared into and be convenient to the molybdenum-base rare earth powder metallurgy sheet alloy process operation technical process that meticulous in-depth is processed into orienting articles and be:

---molybdenum-base rare earth powder metallurgy alloy rolloff blank is put in the hydrogen atmosphere heating furnace of configuration, carries out the first fire heating; Heating-up temperature 1200 ~ 1300 DEG C, heat time 80 ~ 90min, hydrogen flowing quantity>=0.8m ³/ h.After completing heating operation, immediately rolloff blank is laterally put in four roller reversible hot milling rolls, carry out continuous 3 passage lateral shuttle cogging breaking down technical operations; Hot mill rolling power >=400t, roll specification Φ 180 × 400mm, mill speed≤30m/min, on average every time working modulus >=15%.

---after completing the 2nd fiery heating rolling, immediately rolloff blank is put in hydrogen atmosphere annealing furnace, carry out the process of annealing heat retaining operation; Annealing temperature 850 ~ 870 DEG C, annealing high temperature hold time 30 ~ 40min, hydrogen flowing quantity >=0.5m3/h.Reach annealing temperature retention time after power-off, stop hydrogen supply; Rolloff blank takes out after Temperature fall cooling in hydrogen atmosphere annealing furnace.

Next carries out the longitudinal roughing technical operation of multi-pass:

---will complete longitudinal roughing and the cooled rolloff plate of annealing, deliver on plate shearing machine, carry out preliminary cutting edge correction of the flank shape, excise limit more than irregular calendering, can reduce precision cold-rolled power consumption, the tailing reclaiming molybdenum-based rare-earth alloy rolloff plate in time utilizes.

Finally carry out multi-pass precision cold-rolled technical operation:

---the plate through removing surface is longitudinally put on the reversible precise cold milling train of four rollers, carries out first time continuous 3 passages longitudinally round precision cold-rolled; Roll-force >=the 400t of precise cold milling train, roll specification Φ 180 × 400mm, mill speed≤60m/min, on average every time working modulus≤5%.

As shown in Figure 1, technology of preparing unit (VI) is made in described retrofit, comprise Blanking Shaping, elementary grinding, the continuous three kinds of fine processing methods of fine gtinding, molybdenum-base rare earth powder metallurgy sheet alloy rolloff can made is prepared into use user and can the directed molybdenum-base rare earth powder metallurgy alloy disk product process operation technique process used is directly:

---bar shaped plate is put on hydraulic press, by disk hydraulic pressure blanking die, by the specification tolerance of molybdenum-base rare earth powder metallurgy alloy disk goods, uses the circular sheet stock of pliable pressure stamping-out; Stamping-out pressure >=the 100t of the hydraulic press of configuration, rushes circular diameter Φ 25 ~ 110mm, punching circle thickness 0.8 ~ 4.0mm.

---circular sheet stock is put on disk grinder and carry out elementary attrition process; Use common cooling fluid during elementary grinding, allowance 0.06 ~ 0.08mm, lap speed selects 800 ~ 1000r/min.

---the circular sheet stock through elementary grinding is put on disc type precision lapping machine, finally makes fine gtinding processing; Fine gtinding adds man-hour, grinding agent choice for use W20 schmigel+20 ^#machine oil, lap speed selects 1500 ~ 2000r/min.

As shown in Figure 1, described commodity finishing and packing technology of preparing unit (VII), it is the technical standard requirement of dispatching from the factory according to molybdenum-base rare earth powder metallurgy alloy disk goods, carry out clean and tidy, clear up the commercial treatment such as anticorrosion, mark, anticollision packaging, after fulfiling assignment, pin is treated in warehouse-in keeping.

Claims

1. the preparation method of a molybdenum-base rare earth powder metallurgy alloy disk, it is characterized in that: the preparation method of this molybdenum-base rare earth powder metallurgy alloy disk, comprise polynary group of material proportioning (I) of research and design, ultrasonic homogeneous mixture (II), low temperature flexibility hydrostatic pressing (III), retrofit make (VI) technology of preparing unit, and the technical equipment of configuration, the technical parameter of execution, and the industry is published successively sinters sizing (IV), classification multi-pass rolloff (V), commodity finishing and packing (VII) technology of preparing unit; Described ultrasonic homogeneous mixture (II), completed by the ultrasonic homogeneous blending machine of the metal dust configured, the ultrasonic homogeneous blending machine of metal dust, closed circular cone pot structure of container is helped in global design, be made up of mounting bracket (14), taper blending tank tank body (11), blending tank cover (9), realize quick opening and closing of fault fixed operation by mounting flange (10); On blending tank cover (9), be mounted with 6 metal dust atomization chargers (7), dispersed with stirring device (4), safety exhaust (8); On blending tank tank body (11), be mounted with vacuum air pump (6), total terminal box (3), hydrogen gas injection pump (12), discharging opening (13); On the outer wall of blending tank tank body (11), install and fix 3 groups of board-like ultrasonic transducers (5), be connected with automaton (1) by total terminal box (3), bundle conductor (2); Board-like ultrasonic transducer (5), divides position to install along blending tank tank body (11) outer wall with hexagonal angle fixing; Metal dust atomization charger (7), be made up of metal dust holding vessel, high-pressure spray pump, powder jet, be fixed on blending tank cover (9) with a point position, concentric circles 60 ° of angles, wherein 3 pure molybdenum powders loading equivalent and divide equally, all the other 3 are respectively charged into 3 kinds of RE oxide powders, and 4 kinds of metal dusts are alternate position distribution; Dispersed with stirring device (4), be fixed on blending tank cover (9) center, select frequency control motor as driving power source, shaft is mounted with 2 groups and goes to upper and lower rebuilding, each group has 2 hock type dispersed with stirring dishes oppositely installed, and the periphery of each dispersion impeller is mounted with hock; Described low temperature flexibility hydrostatic pressing (III), completed by the heating shaping dies configured and horizontal bidirectional flexible hydraulic harder, heating shaping dies, by right movable pressing board (20), left movable pressing board (25), pressing plate oriented movable groove (19), cover plate (22), base (23), powder loads die cavity (24) and electrical heating elements forms; Heating shaping dies is fixed on harder workbench (29), the right movable pressing board of mould (20) is connected with right oil cylinder pressure head (21), and the left movable pressing board of mould (25) is connected with left oil cylinder pressure head (26); Dextrad pressure densification operation unit is formed by right oil cylinder pressure head (21), right oil cylinder (18), right cylinder bracket (17) and right oil cylinder oil pipe (16), be fixed on harder lathe bed (15) by right cylinder bracket (17), be connected with hydraulic control system case (31) by right oil cylinder oil pipe (16); Left-hand pressure densification operation unit is formed by left oil cylinder pressure head (26), left oil cylinder (28), left cylinder bracket (27) and left oil cylinder oil pipe (30), be fixed on harder lathe bed (15) by left cylinder bracket (27), be connected with hydraulic control system case (31) by left oil cylinder oil pipe (30); It is other that hydraulic control system case (31) is fixed on harder lathe bed (15), and motor, hydraulic oil container, gear oil pump, control valve, distributing valve, overflow valve, safety valve, Monitoring and Controlling instrument, maneuvering and control panel hydraulic work system parts are equipped with in inside; Described retrofit is made (VI), comprises Blanking Shaping, elementary grinding, the continuous fine processing method of fine gtinding, is completed by the hydraulic plate shears configured, hydraulic press, disk grinder, disc type precision lapping machine.

2. the preparation method of a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1, it is characterized in that: polynary group of described material proportioning technology of preparing unit (I), the molybdenum-base rare earth powder metallurgy alloy disk group material component proportioning share adopted, batch to manufacture molybdenum-base rare earth powder metallurgy alloy disk goods gross weight for radix, the proportioning share of various batching component by weight: pure molybdenum powder M ₀93.0 ~ 95.0 parts; Lanthana La ₂o ₃2.2 ~ 2.5 parts; Cerium oxide Ce ₂o ₃1.6 ~ 2.0 parts; Neodymia NdO ₂1.2 ~ 1.5 parts.

3. the preparation method of a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1, it is characterized in that: described ultrasonic homogeneous mixture technology of preparing unit (II), batching component elemental metals powder, solid phase homogeneous mixture is prepared into that constituent element is evenly distributed, preparation technology's job step of the molybdenum-based rare-earth alloy powder of loose particles specification and technical parameter are:

---according to the group material ratio requirement that claim 2 specifies, by the filling rate of metal powder ultrasonic homogeneous blending machine dischargeable capacity 58%, calculate the concrete weight that batching component elemental metals powder feeds intake;

---according to result of calculation, by the electronic-weighing meter of configuration, after Weighing is carried out to batching component elemental metals powder, be respectively charged in corresponding metal dust atomization charger (7);

---start vacuum air pump (6), extract the air in blending tank out, vacuum reaches 12 × 10 ^-3during Pa, close vavuum pump;

---start hydrogen gas injection pump (12) immediately, injecting gas hydrogen in blending tank, gas injection rate reaches 0.12m ³/ m ³time, close gas injection pump;

---start 6 metal dust atomization chargers (7) immediately, 4 kinds of elemental metals powder of batching component are injected in blending tank with continuous spraying while of pink mist, and whole material spray time controling completes in 18 ~ 20min simultaneously;

---meanwhile, start dispersed with stirring device (4), drive to spray with the rotating speed of 1200r/min and flow fast with the two-way route that stirs continuously into all pink mist metal powder granulates in blending tank, realize the homogeneous dispersion to group material component elemental metals powder, be uniformly mixed operation;

---meanwhile, start the supersonic generator in automaton (1), ultrasonic electric energy is coupled on board-like ultrasonic transducer (5), is converted to by board-like ultrasonic transducer (5) and there is 42KH _zfrequency and 4.2w/cm ²the power ultrasonic of the sound intensity, to spraying conduct radiation in all pink mist metal powder granulates in blending tank, the Ultrasonic Radiation time closes supersonic generator after reaching 25 ~ 28min;

---after Ultrasonic Radiation stops, dispersed with stirring device (4) works on 3 ~ 5min, and disperser to be mixed (4) stops operation after 10min, opens discharging opening (13) and takes out the molybdenum-based rare-earth alloy powder that mixture makes.

4. the preparation method of a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1, it is characterized in that: described low temperature flexibility hydrostatic pressing technology of preparing unit (III), molybdenum-based rare-earth alloy powder, pressure densification be prepared into have definite shape size, pressurized general equilibrium, Density Distribution evenly, preparation technology's job step of molybdenum-base rare earth powder metallurgy alloy blank that structural strength is larger and technical parameter be:

---according to density, net weight, shape, the dimensional requirement of molybdenum-base rare earth powder metallurgy alloy disk goods, take into full account the consumption in hydrostatic pressing and sintering type-approval process, scaling loss factor, calculate batch press densification and be shaped and should load to powder the concrete weight loading molybdenum-based rare-earth alloy powder in die cavity (24);

---according to result of calculation, by the electronic-weighing meter of configuration, after Weighing is carried out to molybdenum-based rare-earth alloy powder, load powder and load die cavity (24) interior jolt ramming;

---start the electric heating device of heating shaping dies, the molybdenum-based rare-earth alloy powder be seated in powder filling die cavity (24) is heated to 60 ~ 70 DEG C;

---start horizontal bidirectional flexible hydraulic harder, make left and right two oil cylinders (28), (18) all with the powerful flexible working pressure of the stable and uniform operating rate of 8mm/min and 300MPa, from left and right both direction with equivalent pressure and speed, stable and uniform ground promotes left and right movable pressing board (25), (20) of heating shaping dies, applies powerful pliable pressure to the molybdenum-based rare-earth alloy powder of existing uniform temperature;

---stop mobile when the left and right movable pressing board (25) of heating shaping dies, (20) are advanced to the gear be provided with, now left and right oil cylinder (28), (18) are although can not continue to advance, but still remain the operational pressure of 300MPa, and continue to be applied on molybdenum-based rare-earth alloy powder; After horizontal bidirectional flexible hydraulic harder keeps voltage stabilizing 40min under this operational pressure, take stage by stage unloading pressure means gradually: decompression rate all-the-time stable controls at 6MPa/min; First time unloads and is pressed onto 270MPa, voltage stabilizing 10min; Second time is unloaded and is pressed onto 210MPa, then voltage stabilizing 5min; Third time unloads and is pressed onto 120Mpa, then voltage stabilizing 5min; Press the whole pressure of decompression rate removal of 6MPa/min for 4th time;

5. the preparation method of a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1, it is characterized in that: technology of preparing unit (VI) is made in described retrofit, the retrofit of molybdenum-base rare earth powder metallurgy sheet alloy become preparation technology's job step of molybdenum-base rare earth powder metallurgy alloy disk goods and technical parameter to be:

---molybdenum-base rare earth powder metallurgy sheet alloy is put on hydraulic plate shears, by the molybdenum-base rare earth powder metallurgy alloy disk product specifications size using user's requirement, uses pliable pressure to be cut into bar shaped plate; Configuration hydraulic plate shears cut out thickness 0.8 ~ 4.0mm, cut out length >=1000mm;

---bar shaped plate is put on hydraulic press, by disk hydraulic pressure blanking die, by the molybdenum-base rare earth powder metallurgy alloy disk product specifications size tolerance requirements using user's requirement, uses the circular sheet stock of pliable pressure stamping-out; Stamping-out pressure >=the 100t of the hydraulic press of configuration, rushes circular diameter Φ 25 ~ 110mm, punching circle thickness 0.8 ~ 4.0mm;

---put into by circular sheet stock on disk grinder and carry out elementary attrition process, use common cooling fluid during elementary grinding, allowance 0.06 ~ 0.08mm, lap speed selects 800 ~ 1000r/min;

---the circular sheet stock through elementary grinding is put on disc type precision lapping machine, finally makes fine gtinding processing; Fine gtinding adds man-hour, grinding agent choice for use W20 schmigel+20 ^#machine oil, lap speed selects 1500 ~ 2000r/min, finally makes molybdenum-base rare earth powder metallurgy alloy disk goods.