CN102728838A - Molybdenum-based rare earth oxide powder metallurgical alloy wafer and preparing method thereof - Google Patents

Molybdenum-based rare earth oxide powder metallurgical alloy wafer and preparing method thereof Download PDF

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CN102728838A
CN102728838A CN201110091304XA CN201110091304A CN102728838A CN 102728838 A CN102728838 A CN 102728838A CN 201110091304X A CN201110091304X A CN 201110091304XA CN 201110091304 A CN201110091304 A CN 201110091304A CN 102728838 A CN102728838 A CN 102728838A
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molybdenum
temperature
rare earth
sintering
powder metallurgy
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CN102728838B (en
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陈雄平
陈晨
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Siping Beiwei Molybdenum Industry Limited Company
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SIPING BEIWEI METAL TECHNOLOGY RESEARCH DEVELOPMENT Co Ltd
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Abstract

The invention discloses a molybdenum-based rare earth oxide powder metallurgical alloy wafer and a preparing method thereof. 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

Molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof
Technical field
The present invention relates to a kind of non-ferrous alloy material, relate to a kind of molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof specifically.
Technical background
The molybdenum disk; Because of its fusing point height; Under hot conditions, still have higher intensity and hardness; Still can keep good electric conductivity and conductivity of heat, have fabulous stability, be widely used in production technical field such as Aero-Space, defence and military, metallurgy, electric power, chemical industry, electronics, machinery; In high-tech products such as high-power transmitting tube, high-voltage large current IGCT and rectifier, high temperature thermocouple and protection tube thereof, high-temperature electric resistance furnace heat screen, extraordinary electric light source, be essential basic function material particularly.
The development of molybdenum in China disk is in study, introduce, on the basis with reference to advanced foreign technology, progressively develop and grow up.Last century early sixties; Institution of higher learning and 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 begin to translate the foreign data of introducing relevant molybdenum disk and basic theory etc. propaganda is cognitive and work; And then carried out material behavior research, application conditions analysis, laboratory again in succession and initiative element task such as produced, obtained a series of plentiful and substantial scientific achievements.To last century late nineteen eighties, the early 1990s; More domestic scientific researches, production unit are successively successfully developed out with powder metallurgy process replacement casting method and are processed the rolling again innovative technology that is processed into the molybdenum disk of high temperature molybdenum base; The molybdenum-based rare-earth alloy material of developing out rare earth doped oxide in metal molybdenum is processed the innovative technology of molybdenum disk, makes the manufacturing of molybdenum in China disk goods enter into perfect the raising new stage fast.
Get into 21st century; China's economy grows continuously and fast; Scientific and technological level is progressive fast to be promoted, under the promotion that market demand sharp increase and external product pour in, molybdenum disk goods industry is built in product development development, fabricating technology research and design, commercialization test, application device design production etc. many aspect; All obtained fast development, major scientific and technological achievement continues to bring out.But take a broad view of China's present molybdenum disk industry technology present situation, be mixed at group material proportioning, homogeneous at least, blank is shaped, exist tangible deficiency or weakness aspect four of the special technology equipments etc.
The present invention is through manufacturing the analysis of art survey of status to the molybdenum in China disk; Deficiency and weakness to current existence; Start with from the basic theory analysis; Constitute on the new material three big crucial core technology links at group material proportioning, preparation technology's method, special technology equipment etc. targetedly; Research and design goes out multinomial innovative technology measure, forms a molybdenum-base rare earth powder metallurgy alloy disk technology of preparing that the advanced person is complete, can successfully 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 that the present invention will solve:
The present invention is directed to molybdenum in China disk goods the manufacturing technology exist deficiency and weakness; Research and design goes out in pure molybdenum powder the polynary group of material proportion technique that direct vast scale mixes 3 kinds of RE oxide powders targetedly; Advanced preparation method such as ultrasonic solid phase homogeneous is mixed through taking, low temperature flexibility hydrostatic pressing, sintering typing one by one, the backing of classification multi-pass, retrofit are processed; Form advanced person complete can manufacture out high-performance and high accuracy molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof, and the technical equipment of configuration, the technical parameter of execution.
The technical scheme that technical solution problem of the present invention is taked:
The technical problem that the present invention will solve, intend take research and design go out advanced person complete can manufacture out high-performance and high accuracy molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof, solve.
Molybdenum-base rare earth powder metallurgy alloy disk of research and design of the present invention and preparation method thereof; Comprise that polynary group of material proportioning, ultrasonic homogeneous are mixed, low temperature flexibility hydrostatic pressing, sintering typing one by one, the backing of classification multi-pass, retrofit are processed, technology of preparing unit, commodity finishing and packing 7 road, and the technical equipment of configuration, the technical parameter of execution.
Described polynary group of material proportioning technology of preparing unit is because metal molybdenum has fusing point height (2620 ℃), under hot conditions, still has higher intensity and hardness, still has excellent electrical and thermal conductivity and good stable property.But the recrystallization temperature of metal molybdenum lower (1100 ℃), again after the crystallization molecular organization structure to change equiax crystal into granular by fibrous, become network, and along with the temperature of environment for use raises, grainiess is grown up sharply vertically; Therefore, metal molybdenum is being deposited the brittle failure easily of annealing back, and mechanical and physical performances such as tension, surrender, extension are relatively poor, major defects such as saw lumber shaping difficulty; And the molecular structure of rare earth element is the chain crystal grain of arranging vertically of growing up; Be the long brilliant chain bridging arrangement state of dovetail shaped again after the crystallization; Under hot conditions, still have stronger sagging resistance and creep properties preferably; Can have stronger inhibitory action to the grain growth of metal molybdenum after adding chemical combination, can improve the recrystallization temperature of metal molybdenum, thereby can improve the mechanical and physical performance of metal molybdenum; Simultaneously; Rare earth element all has stronger dispersion-strengthened action again, can form film at the grain surface of metal molybdenum, performance " embedding effect " behind the interpolation chemical combination; Can stop gas phase water and oxide to deposit at the metal molybdenum grain surface; Form dispersoid particle, and can pass through dispersoid particle and metal molybdenum molecular network lattice structure generation dislocation effect, thereby the crystal grain specific area of increase metal molybdenum, crystal grain thinning granularity, inhibition grain growth, delay crystallization again and be inclined to; Improve the recrystallization temperature of metal molybdenum, improve the mechanical and physical performance of molybdenum-based rare-earth alloy material material and shape manufacturability.
The proportioning share of the various batching components of molybdenum-base rare earth powder metallurgy alloy disk: with a batch manufacturing molybdenum-base rare earth powder metallurgy alloy disk goods gross weight is radix, and the proportioning share of various batching components is by weight: pure molybdenum powder (M 0) [93.0～95.0] part; Lanthana (La 2O 3) [2.2～2.5] part; Cerium oxide (Ce 2O 3) [1.6～2.0] part; Neodymia (NdO 2) [1.2～1.5] part.
Batching component granularity: the powder size of various batching components all≤4 μ m.
Batching component purity: the purity of various batching components 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: select to use the thermal coefficient of expansion of 3 kinds of rare earth elements all very approaching with metal molybdenum, under the hot operation condition, can keep the non-deformability with metal molybdenum parent basic synchronization.Select 3 kinds of rare earth elements of use, high melt point and boiling point are all arranged, La has 2300/4200 ℃, and Ce has 2272/4050 ℃, and Nd has 2715/4840 ℃; Under high temperature (≤1800 ℃) condition of work not can with metal molybdenum parent phased soln, can keep the excellent specific property of metal molybdenum parent preferably.Select 3 kinds of rare earth elements of use, not only have rare earth element total good resistance droop and creep properties, and can have different deep drawing qualities and high plasticity again separately, have cold-resistant preferably fragility and non-oxidizability; Can play a significant role with the processing serviceability to improving molybdenum base material material, particularly mechanical and physical performance after adding chemical combination.Select to confirm to mix 3 kinds of rare earth oxides simultaneously, it can be supported each other, can fully represent characteristic separately again, more can give full play of the dispersion-strengthened action of rare earth element metal molybdenum with larger proportion.
The described ultrasonic homogeneous technology of preparing unit that is mixed is because ultrasonic wave has extremely strong penetration capacity, and fabulous conductibility is also arranged in the solid medium; Ultrasonic wave conducts in the solid medium, can cause the medium particulate and get into vibrational state, produces and transmit powerful energy, impels the medium particulate constantly to carry out displacement movement to antinode or node, forms displacement effect; Though shift length is little, very big with the ultrasonic frequency vibratory square acceleration that is directly proportional, even can be above several ten thousand times of acceleration of gravity; So huge acceleration energy is enough to cause the medium particulate and strong collision takes place, break, move the isostructuralism variation.Cooperate the employing mechanical atomization to spray simultaneously and stir mixed technology, each metal dust of organizing the material component is advanced in the ultrasonic homogeneous compounder of metal dust by mixed ratio while continuous injection with the dust cloud state; Lean on the high speed rotary motion of dispersed with stirring device; Make to be arranged in the high-frequency that the dispersed with stirring web obtains high linear velocity and cuts bump metal dust particulate along last hock, thereby produce dynamic powers such as the extremely strong high speed shear of metal dust particulate, centrifugal extruding; This extremely strong dynamic potential energy matches with the displacement effect that power ultrasonic produces again, is enough to increase quickening metal dust particulate and breaks, moves, collides the isostructuralism variation.Power ultrasonic and this constructive variations that machinery is mixed and combines powder particle is produced are enough to refinement, dispersion, the homogeneous of each batching component metal dust particulate are played a great role, and also can effectively destroy the distinctive reunion adhesion energy of powder particle; Using ultrasound solid phase homogeneous mixed technology; The component of respectively preparing burden to being the solid state powder shape is implemented the operation of refinement homogeneous dispersion; Just can refinement respectively the prepare burden crystallite size of component; Strengthen the homogeneous dispersion degree of the component of respectively preparing burden, the growth conditions of thick fragility crystal grain in the component that suppresses respectively to prepare burden, thereby for improving the molybdenum base material material condition that lays a good foundation that improves.
The ultrasonic homogeneous technology of preparing unit that is mixed is accomplished by the ultrasonic homogeneous compounder of metal dust of original creation design.
The ultrasonic homogeneous compounder of metal dust, global design are helped sealing circular cone jar type structure of container, are made up of mounting bracket, taper blending tank tank body, blending tank cover, realize quick opening and closing of fault fixed operation through mounting flange; On the blending tank cover, be mounted with operation parts such as 6 metal dust atomization chargers, dispersed with stirring device, safety exhaust; On the 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, install and fix 3 groups of board-like ultrasonic transducers along the tank body circumference with hexagonal angle branch position, be connected with automaton through total terminal box, bundle conductor.
Board-like ultrasonic transducer; Can convert the ultrasonic electric energy that supersonic generator produces to high-frequency mechanical vibration ripple with suitable power energy; Penetrate in the dust cloud shape metal dust of blending tank tank skin in blending tank and conduct; Make the metal dust particulate produce dither, form displacement effect, produce and transmit huge energy.
Vacuum air pump and hydrogen gas injection pump are fixed on the upper and lower of blending tank tank body respectively.Because of rare earth element all has the 4f electronic structure; And electronegativity is little; Very easily be corroded, particularly high-purity simple substance pulverulence is very responsive to airborne oxygen, for guaranteeing the purity of rare earth metal powder in mixing operation process; Take to vacuum environment filling can be preferential and the hydrogen of oxygen chemical combination as safeguard measure, vacuum suction vacuum: 10 * 10 -3Pa, hydrogen gas injection rate: 0.12m 3/ m 3
The 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 the blending tank cover with branch position, 60 ° of angles of concentric circles; The pure molybdenum powder of 3 equivalent of packing into wherein; All the other 3 are respectively charged into other 3 kinds of RE oxide powders; Distribution is put in 4 kinds of metal dust submission displacements, can 4 kinds of metal dusts of group material component be advanced to get into simultaneously in the blending tank solid phase homogeneous dispersion with the dust cloud state by the mixed ratio continuous injection and stir the operation that is mixed.
The dispersed with stirring device is fixed on the blending tank cover center.Select frequency control motor as driving power source, can make the adjustment that different rotating speeds changes according to the needs that are mixed of different phase; The dispersed with stirring device is employed in and is mounted with 2 groups on the shaft and goes to upper and lower double-deck the layout, and each group all has 2 reverse hock type dispersed with stirring dishes of installing, and all is mounted with the structural arrangement form of some hocks on the edge of each dispersion impeller.When carrying out the dispersed with stirring operation; Because the effect of the rotation of the high speed of dispersed with stirring device and 2 groups of reverse hock type dispersion impellers on the card of hock type dispersion impeller, all can produce one extremely strong axial attraction separately; Dust cloud shape metal dust is sucked from the axial relative direction of card simultaneously fast; Again from the centre of 2 groups of dispersion impeller dishes back of the body fast to around flow out, run into the blending tank tank skin after, both direction flows up and down respectively; Form the two-way route that stirs continuously and flow fast thereby driven whole dust cloud shape metal dusts in the blending tank, eliminated homogeneous dispersion, mixed blind area or dead angle that operation possibly exist.Simultaneously; Lean on the high speed rotary motion of dispersed with stirring device; Make the some hocks of design arrangement at dispersed with stirring dish periphery; Can both obtain the high-frequency of high linear velocity and the vaporific metal dust of cutting bump, thereby produce dynamic powers such as extremely strong high speed shear of metal dust particulate and centrifugal extruding.
The ultrasonic homogeneous technology of preparing unit that is mixed; Be the elemental metals powder of manufacturing the required various batching constituent elements of molybdenum-base rare earth powder metallurgy alloy disk; In the ultrasonic homogeneous compounder of metal dust of configuration; Through power ultrasonic vibration displacement, atomized spray, homogeneous dispersion, the engineering means such as mix, the solid phase homogeneous is mixed into that constituent element is evenly distributed, the molybdenum-based rare-earth alloy powder technology operation process of loose particles standard.
The ultrasonic homogeneous technology of preparing unit that is mixed, preparation technology's operation technique process is:
---according to the specification requirement of group material proportioning; Molybdenum-base rare earth powder metallurgy alloy disk goods gross weight with batch production is a radix; Press the filling rate of the ultrasonic homogeneous compounder of metal powder dischargeable capacity 58%, accurately calculate the concrete weight that various batching component elemental metals powder feed intake.
---according to result of calculation, through the electronic-weighing meter of configuration, various batching component elemental metals powder distinguish Weighing after, be respectively charged in the metal dust atomization charger that is arranged on correspondence on the ultrasonic homogeneous compounder of metal dust.
---start vacuum air pump, extract the air in the 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 3The time, close the gas injection pump.
---start 6 metal dust atomization chargers immediately simultaneously; Under the effect of high-pressure spray pump, through powder jet, advance the elemental metals powder of 4 kinds of batching constituent elements in the blending tank with dust cloud shape while continuous injection by mixed ratio; All the spray material time is controlled in 18～20min and accomplishes.
---meanwhile start the dispersed with stirring device; Rotating speed with 1200r/min rotates at a high speed; Driving all metal powder granulates of dust cloud shape that spray in the blending tank flows with the two-way route that stirs continuously fast; And bump cutting and the dispersion of accepting to be installed in dynamic powers such as the high-speed cutting of dispersed with stirring dish periphery hock, centrifugal extruding mix operation; Match with dither, displacement effect that power ultrasonic forms, accomplish homogeneous dispersion, mix operation multiple elemental metals powder.
---meanwhile start the supersonic generator in the automaton, to board-like ultrasonic transducer, convert ultrasonic couple electrical energy by board-like ultrasonic transducer to and have 42KHZ frequency and 4.2w/cm 2The power ultrasonic of the sound intensity; All metal powder granulates conduct radiation of dust cloud shape in blending tank is advanced in injection; Cause dither and displacement effect; Stir the dynamic potential energy that forms with mechanical dispersion and match, make metal powder granulates produce displacement, the isostructuralism of colliding, break variation, just can give play to powerful crystal grain thinning granularity, strengthen the effect of homogeneous dispersion degree.After the ultrasonic wave radiated time reaches 25～28min, close supersonic generator.
---after the ultrasonic wave radiation stops, the dispersed with stirring device 3～5min that works on; Wait to close the dispersed with stirring device and stop operation behind the 10min, open discharging opening, take out the molybdenum-based rare-earth alloy powder that homogeneous is mixed and processes.
Described low temperature flexibility hydrostatic pressing technology of preparing unit; Be because cryogenic forming is the advanced and sophisticated technology of powder metallurgy industry; Through having the shaping dies of low-temperature heat function; When the molybdenum-based rare-earth alloy powder is heated to 60～70 ℃, can in alloy powder, form bigger activation energy.This activation energy can improve mechanical interlocking and surface atom attraction between the alloy powder particle, increases the intensity of shaping base substrate; Can improve the flowability of alloy powder particle, increase the density and the homogeneous degree of shaping base substrate; Can also improve the oxygen reduction speed of rare earth oxide, avoid or reduce occurring tissue defects such as crackle, bubble, shrinkage porosite in the shaping base substrate.Because the fine and close power resources that are shaped of alloy powder are to rely on pressure fine and close, require this pressure power must be able to make alloy powder particle all produce brittle fracture after, could form new body again; But, if uneven to the alloy powder applied pressure, or insufficient pressure, time are not enough, will strain only take place some alloy powder particle, and plastic deformation does not also take place, and more do not produce brittle fracture; If this moment pressure relief, bounce-back just possibly take place or restore to the original state in these powder particles that strain only takes place, therefore neomorph is inner expansion, shrinkage porosite will occur, perhaps produces underbead crack, stays serious hidden danger of quality.Therefore, must guarantee that the isostasy of exerting pressure is powerful lasting, make alloy powder particle all produce brittle fracture, qualified neomorph is formed in densification.
Low temperature flexibility hydrostatic pressing technology of preparing unit is accomplished by the heating shaping dies and the horizontal bidirectional flexible hydraulic harder of original creation design.
The heating shaping dies is made up of left and right sides movable pressing board, pressing plate loose slot, cover plate, base, powder filling die cavity and electrical heating elements.The heating shaping dies is fixed on the hydraulic pressure harder workbench, and the right movable pressing board of mould is connected with right oil cylinder pressure head, and mould left side movable pressing board is connected with left oil cylinder pressure head; Form the closely knit operation unit of dextrad pressure by right oil cylinder pressure head, right oil cylinder, right cylinder bracket and right oil cylinder oil pipe, be fixed on the hydraulic pressure harder workbench, be connected with the hydraulic operation control cabinet through right oil cylinder oil pipe through right cylinder bracket; Form the closely knit operation unit of left-hand pressure by left oil cylinder pressure head, left oil cylinder, left cylinder bracket and left oil cylinder oil pipe, be fixed on the hydraulic pressure harder workbench, be connected with the hydraulic operation control cabinet through left oil cylinder oil pipe through left cylinder bracket.The hydraulic operation control cabinet is fixed on by the hydraulic pressure harder lathe bed, and 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, manipulation control panel are equipped with in inside.
Low temperature flexibility hydrostatic pressing technology of preparing unit; Be the molybdenum-based rare-earth alloy powder through the engineering measure such as exert pressure of static pressure such as cryogenic forming mold heated, bidirectional flexible, pressure is fine and close become to have definite shape size, pressurized general equilibrium, Density Distribution evenly, molybdenum-base rare earth powder metallurgy alloy blank technical operation process that structural strength is bigger.
Low temperature flexibility hydrostatic pressing technology of preparing unit, preparation technology's operation technique process is:
---according to concrete needs such as the desired density of molybdenum-base rare earth powder metallurgy alloy disk goods, net weight, shape, size; Take into full account factors such as consumption in hydrostatic pressing and sintering type-approval process, scaling loss, shaping porosity, sintering shrinkage, accurately calculate the densification of this batch pressure and be formed in the concrete weight of molybdenum-based rare-earth alloy powder that the mold cavity planted agent loads.
---according to result of calculation, through the electronic-weighing meter of configuration, the molybdenum-based rare-earth alloy powder carried out Weighing after, jolt ramming in the cryogenic forming mold cavity of packing into.
---start the electric heating device of cryogenic forming mould, the molybdenum-based rare-earth alloy powder that is contained in the cryogenic forming mold cavity is heated to 60～70 ℃.
---start horizontal bidirectional flexible hydraulic harder; The static pressure such as bidirectional flexible that rely on hydraulic system the to have function of exerting pressure; Make left and right two oil cylinders can both be with the stable and uniform operating rate of 8mm/min and the powerful flexible working pressure of 300MPa; From pressure and the speed of left and right both direction to be equal to, stable and uniform ground promotes the left and right movable pressing board of cryogenic forming mould, and the molybdenum-based rare-earth alloy powder that has uniform temperature is applied powerful pliable pressure; Fixed form around the cryogenic forming mould; Under the impressed pressure effect, form the reaction force that equates with this pressure; Around the molybdenum-based rare-earth alloy powder, exert pressure simultaneously; Make molybdenum-based rare-earth alloy powder in the cryogenic forming mold cavity receive simultaneously each to brute force exert pressure, and make each to the pressurized general equilibrium.
---the left and right movable pressing board of cryogenic forming mould, stop to move when being advanced to the gear that is provided with, though this moment, left and right oil cylinder can not continue to advance, still keeping the operational pressure of 300MPa, and continuing to be applied on the molybdenum-based rare-earth alloy powder; Horizontal bidirectional flexible hydraulic harder is after keeping voltage stabilizing 40min under this operational pressure, and take to reduce pressure gradually stage by stage unloading pressure means: release speed all-the-time stable is controlled at 6MPa/min; Unload for the first time and be pressed onto 270MPa, voltage stabilizing 10min; Unload for the second time and be pressed onto 210MPa, again voltage stabilizing 5min; Unload for the third time and be pressed onto 120Mpa, again voltage stabilizing 5min; Press the whole pressure of release speed removal of 6MPa/min for the 4th time.
---demoulding, take out the fine and close molybdenum-base rare earth powder metallurgy alloy blank that is shaped of pressure.
The described typing of sintering one by one technology of preparing unit; Be through taking in hydrogen atmosphere, to carry out PM technique means such as low-temperature bake, middle temperature presintering, the typing of intermediate frequency high temperature sintering continuously one by one; After making the molybdenum-base rare earth powder metallurgy alloy blank shrink great variety such as densification, intensity increase, stable raisings of physical and chemical performance, be prepared into the molybdenum-base rare earth powder metallurgy alloy backing blank technical operation process that no dirtyization of sizing in surface, the no hierarchical crack in inside, tissue density are evenly distributed.
Sintering typing technology of preparing unit disposes 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 one by one.
Sintering typing technology of preparing unit one by one, preparation technology's operation technique process is:
At first carry out the low-temperature bake technical operation:
---the molybdenum-base rare earth powder metallurgy alloy blank is put in the hydrogen atmosphere low-temperature bake stove; Use lower temperature to carry out low-temperature bake; Can make bond strength increase between the molybdenum-based rare-earth alloy particle in the blank, gravitational force between atoms increases on the link surface, makes to take place between alloying pellet to attract bonding to fix; Can eliminate simultaneously the part elasticity internal stress of dissolving blank when pressure is fine and close to be shaped, the most of gas and the moisture content of blank absorption is got rid of in volatilization.The heating rate of low-temperature bake is stable to be controlled at 10 ℃/min (± 2 ℃), and the highest baking temperature is controlled at 480 ℃ (± 5 ℃), all stoving times be controlled at 100min (± 10min); Hydrogen flowing quantity is stable in the bake process is controlled at>=0.8m 3/ h.Low-temperature bake cuts off the power supply after reaching stoving time, leans on natural cool-down method cooling in the stove; When treating that temperature is reduced to 120 ℃ in the stove, will toast blank immediately and be transferred to and carry out the intermediate sintering temperature technical operation in the intermediate sintering temperature stove.
Warm presintering technical operation during next carries out:
---the baking blank that will have 120 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate sintering temperature stove that is preheating to equal temperature; Use sufficient temp to carry out intermediate sintering temperature, make to produce big activation energy in the blank, let the atom amplitude of molybdenum-based rare-earth alloy particle strengthen; Abundant atom is entered in the atom graviational interaction scope; Impel multiple migration forms such as atom passes through evaporation, diffusion, flows, cohesion, between the molybdenum-based rare-earth alloy particle, form crystal grain boundary, and progressively move to granule interior; The intergranular reduced distances of molybdenum-based rare-earth alloy, porosity dwindle, density increases thereby make, and finally make the volume contraction of molybdenum-base rare earth powder metallurgy alloy blank; The oxide that can make the molybdenum-based rare-earth alloy particle surface simultaneously is by reduction fully, and the gas of blank absorption, moisture content quilt are all got rid of volatilization, and the internal stress that blank forms in the fine and close shaping of pressure is thoroughly eliminated to be dissolved.The stable 15 ℃/min (± 2 ℃) that is controlled at of the heating rate of intermediate sintering temperature, senior middle school temperature sintering temperature is controlled at 980 ℃ (± 5 ℃), all the intermediate sintering temperature times be controlled at 150min (± 10min) in, hydrogen flowing quantity is stablized and is controlled at>=1.5m in the sintering process 3/ h.Intermediate sintering temperature cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove; When treating that temperature is reduced to 250 ℃ in the stove, the intermediate sintering temperature blank is transferred to carries out the operation of high temperature sintering shaping technology in the intermediate frequency high temperature sintering furnace immediately.
Carry out the operation of high temperature sintering shaping technology at last:
---the intermediate sintering temperature blank that will have 250 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate frequency high temperature sintering furnace that is preheating to equal temperature; Use higher temperature to carry out the high temperature sintering typing of long period; The blank atom diffusion is fully carried out with flowing; 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 typing is divided into 3 stages: from 250 ℃ of temperature, with the heating rate of 15 ℃/min (± 2 ℃) 20min that heats up continuously, make furnace temperature reach 550 ℃, steady temperature 10min; With the programming rate of 10 ℃/min (± 2 ℃) 30min that heats up continuously, make furnace temperature reach 850 ℃, steady temperature 35min again; Be warmed up to 1225 ℃ of the highest controlling values (± 5 ℃) of intermediate frequency high temperature sintering temperature more continuously with the programming rate of 15 ℃/min (± 2 ℃); On this temperature line, steady temperature sintering 120min, make whole sintering times of high temperature intermediate frequency sintering typing be controlled at 240min (± 10min).In the intermediate frequency high temperature sintering type-approval process, hydrogen flowing quantity is stable to be controlled at>=2m 3/ h.The intermediate frequency high temperature sintering cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove; After temperature is reduced to normal temperature in the stove, take out the molybdenum-base rare earth powder metallurgy alloy backing blank of processing.
Described classification multi-pass backing technology of preparing unit; Be through on general roll off plant equipment, taking horizontal cogging breaking down, vertically roughing, accurate cold rolling five equilibrium level multi-pass backing technological means; Molybdenum-base rare earth powder metallurgy alloy backing blank can both be accomplished to the goods form transformation aspect many at interior tissue, geometry, mechanical and physical performance etc., be prepared into the molybdenum-base rare earth powder metallurgy sheet alloy technical operation process that orienting articles is processed in meticulous in-depth of being convenient to.
Classification multi-pass backing technology of preparing unit disposes 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 backing technology of preparing unit, preparation technology's operation technique process is:
At first carry out the horizontal cogging breaking down of multi-pass technical operation:
---put molybdenum-base rare earth powder metallurgy alloy backing blank in the hydrogen atmosphere heating furnace into, carry out the first fire heating; 1200～1300 ℃ of heating-up temperatures, heat time heating time 80～90min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls, carried 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%.
---accomplish the first fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere heating furnace again, carry out the second fire heating; 1100～1200 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls again, still used≤mill speed of 30m/min, carry out taking turns 3 passage lateral shuttle cogging breaking down operations more continuously; Average every time working modulus>=20%.
---accomplish the 2nd fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere annealing furnace, the heat retaining operation of annealing is handled; 850～870 ℃ of annealing temperatures, annealing high temperature retention time 30～40min, hydrogen flowing quantity>=0.5m 3/ h.Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply; The backing blank is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace.
Design arrangement is carried out the horizontal cogging breaking down of multi-pass operation, on rolling direction, all selects cross rolling, can reduce the anisotropy on blank tissue and the performance, improves the blank horizontal plastic property; Select to adopt higher heating-up temperature and big pass reduction; Can make blank obtain big draught pressure; Guarantee that the blank atom gets into the metallic bond gravisphere, the raising of blank intercrystalline bond strength, density are increased, can avoid occurring mass defects such as interlayer, crackle; Select to adopt higher anneal temperature and long annealing temperature retention time, can make blank obtain more processing texture structure, avoid the crystallization again of metal molybdenum to take place, can effectively eliminate the internal stress of blank, improve the room temperature mechanical physical property after the blank backing becomes sheet material.
Next carries out the vertical roughing technical operation of multi-pass:
---the backing blank that will pass through the cogging breaking down is put in the hydrogen atmosphere heating furnace, carries out the first fire heating; 950～1050 ℃ of heating-up temperatures, heat time heating time 70～80min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, vertically put the backing blank on the four roller reversibly hot milling trains immediately, carry out continuous 3 passages and vertically come and go the roughing operation; Hot mill rolling power>=400t, roll specification Φ 180 * 400mm, mill speed≤45m/min, on average every time working modulus≤12%.
---accomplish the first fiery heating rolling after, put the backing blank again in the hydrogen atmosphere heating furnace immediately, carry out the 2nd fire heating; 900～1000 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, put the backing blank again on the four roller reversible hot milling rolls immediately, still use≤mill speed of 45m/min, carry out taking turns 3 passages more continuously and vertically come and go the roughing operation, on average every time working modulus≤10% is rolled into the backing plate.
---accomplish the 2nd fiery heating rolling after, immediately the backing plate is put in the hydrogen atmosphere annealing furnace, the heat retaining operation of annealing is handled; 850～870 ℃ of annealing temperatures, annealing high temperature retention time 50～60min, hydrogen flowing quantity>=0.5m 3/ h.Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply; The backing plate is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace.
---will accomplish vertical roughing and the cooled backing plate of annealing; Deliver on the plate shearing machine, tentatively cut the limit correction of the flank shape, excise the surplus limit of irregular calendering; Can reduce accurate cold rolling power consumption, in time reclaim the tailing utilization of molybdenum-based rare-earth alloy backing plate.
The vertical roughing operation of multi-pass is arranged in design; On rolling direction, all select vertically rolling; Can cooperatively interact with the horizontal breaking down of cogging, form a kind of switching-over tandem rolling technical method, the slab interior tissue is distributed to reasonable direction; Anisotropy is obviously reduced, and can make rolling plate in vertical, the horizontal two-way better technical performance that can both obtain unification; Select to adopt lower heating-up temperature and less pass reduction, the geometry of backing plate can be finalized the design almost, acquired excellent mechanical physical property is kept stable preferably.
Carry out the accurate cold rolling technical operation of multi-pass at last:
---thoroughly clear up carrying out accurate cold rolling backing panel surface, hard foreign material such as the burr of avoiding adhering to, decortication cause impression, draw mass defects such as mark panel surface.After accomplishing prune job, smear very thin one deck cold-rolling lubricant in panel surface with cotton yarn.
---the backing plate that will pass through removing surface is vertically put on the reversible precise cold milling train of four rollers, carries out the first time continuous 3 passages and vertically comes and goes accurate cold rolling; 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 accomplish the plate of the 1st precision after cold rolling, carry out again thoroughly cleaning of surface; Smear cold-rolling lubricant with cotton yarn in panel surface once more.
---will vertically put into once more on the reversible precise cold milling train of four rollers through the plate of the 2nd subsurface cleaning, still with the mill speed of≤60m/min, carry out continuously again 3 passages vertically come and go accurate cold rolling, average every time working modulus≤2%; The molybdenum-base rare earth powder metallurgy sheet alloy is processed in final backing, and reaches the gauge tolerance standard of technical papers regulation.
The technology of preparing unit is processed in described retrofit: be through on the special-purpose machinery process equipment, taking retrofits such as blanking shaping, elementary grinding, precise finiss to process technological means, manufacturing out the technical operation process of molybdenum-base rare earth powder metallurgy alloy disk goods.
The technology of preparing unit is processed in retrofit, disposes current techique equipments such as hydraulic plate shears, hydraulic press, disk grinder, disc type precision lapping machine.
The technology of preparing unit is processed in retrofit, and preparation technology's operation technique process is:
---sheet material is put on the hydraulic plate shears,, used pliable pressure to be cut into the bar shaped plate by the molybdenum-base rare earth powder metallurgy alloy disk goods specification that uses customer requirements; The hydraulic plate shears of configuration cut out thickness 0.8～4.0mm, cut out length >=1000mm.
---the bar shaped plate is put on the hydraulic press,, pressed the specification tolerance of molybdenum-base rare earth powder metallurgy alloy disk goods, use the circular sheet stock of pliable pressure stamping-out through disk hydraulic pressure blanking die; Stamping-out pressure >=the 100t of hydraulic press towards circular diameter Φ 25～110mm, dashes circle thickness 0.8～4.0mm.
---circular sheet stock put into carry out elementary attrition process on the disk grinder; Use common cooling fluid during elementary grinding, allowance 0.06～0.08mm, lap speed is selected 800～1000r/min.
---the circular sheet stock that will pass through elementary grinding is put on the disc type precision lapping machine, finally processes fine gtinding processing; Fine gtinding adds man-hour, and grinding agent selects to use W20 schmigel+20 #Machine oil (proportioning 1: 15～20), lap speed is selected 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 commercializations such as clean and tidy, cleaning, anticorrosion, sign, anticollision packing and handles; Pin is treated in the warehouse-in keeping after accomplishing.
Advantage that the present invention has and the effect that reaches:
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 distinctive dispersion-strengthened action of metal molybdenum and embedding effect; Intensity, toughness and the plasticity of molybdenum-based rare-earth alloy material material have been improved effectively; Improve the processing serviceability, expanded range of application.
2, the ultrasonic solid phase homogeneous of the research and design of the present invention innovative technology that is mixed; Make full use of power ultrasonic and can produce high-frequency, high strength, high-energy mechanical oscillation function and displacement effect, spray the technology of mixing with traditional mechanical atomization and match, effectively refinement the crystallite size of batching group element material; Strengthened the homogeneous dispersion degree; Destruction has been cleared up the reunion adhesion energy that powder particle very easily produces, and has simplified preparation technology, has reduced 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; Rely on the static pressure such as bidirectional flexible of low-temperature heat function and the harder hydraulic system of the shaping dies function of exerting pressure; Make the molybdenum-based rare-earth alloy powder particle can on all directions, accept powerful equalization stable equivalent pressure simultaneously, accomplish developing to complete brittle fracture, become the fine and close neomorph of pressure from strain; Solved and often existed serious hidden danger of quality problem such as expansion, shrinkage porosite, crackle in the fine and close shaping base substrate of traditional liquid pressure medium; Improved the material quality of molybdenum original washing powder smelting rare earth alloy blank effectively, created advantage, the robust techniques quality assurance is provided for follow-up saw lumber in-depth processing.
4, the continuous sintering one by one of research and design of the present invention typing innovative technology; After molybdenum-based rare-earth alloy powder process low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering typing continuous sintering processing; Can make that the shaping base substrate becomes that 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 be with reference to the new technology of using for reference.
Description of drawings
Accompanying drawing 1: molybdenum-base rare earth powder metallurgy alloy disk preparation method technology path sketch map.
Accompanying drawing 2: the ultrasonic homogeneous compounder of metal dust structural principle sketch map.
Accompanying drawing 3: horizontal bidirectional flexible hydraulic harder structural principle sketch map.
The specific embodiment
Shown in accompanying drawing 1; Molybdenum-base rare earth powder metallurgy alloy disk of the present invention and preparation method thereof; Comprise that polynary group of material proportioning (I), ultrasonic homogeneous are mixed (II), low temperature flexibility hydrostatic pressing (III), (VI), technology of preparing unit, commodity finishing and packing (VII) 7 road are processed in sintering typing (IV), classification multi-pass backing (V), retrofit one by one, and the technical equipment of configuration, the technical parameter of execution.
Shown in accompanying drawing 1; Described polynary group of material proportioning technology of preparing unit (I); Confirm the proportioning share of various groups of material components of molybdenum-base rare earth powder metallurgy alloy disk; With a batch manufacturing molybdenum-base rare earth powder metallurgy alloy disk goods gross weight is radix, and the proportioning share of various batching components is by weight: pure molybdenum powder (M 0) [93.0～95.0] part; Lanthana (La 2O 3) [2.2～2.5] part; Cerium oxide (Ce 2O 3) [1.6～2.0] part; Neodymia (NdO 2) [1.2～1.5] part.
Batching component granularity: the powder size of various batching components all≤4 μ m.
Batching component purity: the purity of various batching components all>=99.9%; Total impurities adds up to all≤500 μ g/g.
Shown in accompanying drawing 1, accompanying drawing 2, the described ultrasonic homogeneous technology of preparing unit (II) that is mixed is accomplished by the ultrasonic homogeneous compounder of metal dust of original creation design.The ultrasonic homogeneous compounder of metal dust, global design are helped sealing circular cone jar type structure of container, are 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 through mounting flange (10); On blending tank cover (9), be mounted with 6 metal dust atomization chargers (7), dispersed with stirring device (4), safety exhaust operation parts such as (8); (on 11, be mounted with vacuum air pump (6), total terminal box (3), hydrogen gas injection pump (12), discharging opening (13) at the blending tank tank body; 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) through total terminal box (3), bundle conductor (2).
Board-like ultrasonic transducer (5); Install and fix with hexagonal angle branch position along blending tank tank body (11) outer wall; Can be conducting in the dust cloud shape metal dust of the power ultrasonic with suitable power energy in blending tank is advanced in injection; Make 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 the blending tank cover (9) with branch position, 60 ° of angles of concentric circles; The pure molybdenum powder of 3 equivalent of packing into wherein; All the other 3 are respectively charged into 3 kinds of RE oxide powders, make 4 kinds of metal dust submission displacements put distribution, can 4 kinds of metal dusts of group material component be advanced in the blending tank by mixed ratio while continuous injection with the dust cloud state.Dispersed with stirring device (4) is fixed on blending tank cover (9) center, selects frequency control motor as driving power source, can make the adjustment that different rotating speeds changes according to the needs that are mixed of different phase; Dispersed with stirring device (4) is mounted with 2 groups and goes to upper and lower double-deck the layout on shaft, each group all has 2 reverse hock type dispersed with stirring dishes of installing, and the periphery of each dispersion impeller all is mounted with some hocks; When carrying out the dispersed with stirring operation; Because the effect of the rotation of the high speed of dispersed with stirring device (4) and 2 groups of reverse hock type dispersion impellers; On the card of each hock type dispersion impeller, all can produce one extremely strong axial attraction; Dust cloud shape metal dust is sucked from the axial relative direction of card simultaneously fast, again from the centre of 2 dispersion impeller dishes back ofs the body fast to around flow out, run into behind the blending tank tank skin can be respectively up and down both direction flow; Form the two-way route that stirs continuously and flow fast thereby driven whole dust cloud shape metal dusts in the blending tank, eliminated homogeneous dispersion, mixed blind area or dead angle that operation possibly exist; Simultaneously; Lean on the high speed rotary motion of dispersed with stirring device (4); Make the some hocks of design arrangement at dispersed with stirring dish periphery; Can both obtain the high-frequency of high linear velocity and cutting bump atomized metal pow der, thereby produce dynamic powers such as extremely strong high speed shear of metal dust particulate and centrifugal extruding.
The ultrasonic homogeneous technology of preparing unit (II) that is mixed, the elemental metals powder of various batching components, the solid phase homogeneous is mixed and is prepared into that component is evenly distributed, the molybdenum-based rare-earth alloy powder technology operation technique process of loose particles standard is:
---according to the specification requirement of group material proportioning; Molybdenum-base rare earth powder metallurgy alloy disk goods gross weight with batch production is a radix; Press the filling rate of the ultrasonic homogeneous compounder of metal powder dischargeable capacity 58%, accurately calculate the concrete weight that various batching component elemental metals powder feed intake.
---according to result of calculation, through the electronic-weighing meter of configuration, various batching component elemental metals powder distinguish Weighing after, be respectively charged in the metal dust atomization charger (7) of correspondence.
---start vacuum air pump (6), extract the air in the 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 3The time, close the gas injection pump.
---start 6 metal dust atomization chargers (7) immediately simultaneously; Under the effect of high-pressure spray pump, through powder jet, advance the elemental metals powder of 4 kinds of batching components in the blending tank with dust cloud shape while continuous injection by mixed ratio; All the spray material time is controlled in 18～20min and accomplishes.
---meanwhile start dispersed with stirring device (4); Rotating speed with 1200r/min rotates at a high speed; Driving all dust cloud shape metal powder granulates that spray in the blending tank flows with the two-way route that stirs continuously fast; And bump cutting and the dispersion of accepting to be installed in dynamic powers such as the high-speed cutting of dispersed with stirring dish periphery hock, centrifugal extruding mix operation; Match with dither, displacement effect that power ultrasonic forms, accomplish homogeneous dispersion, mix operation multiple elemental metals powder.
---meanwhile, the supersonic generator in the startup automaton (1) arrives ultrasonic couple electrical energy on the board-like ultrasonic transducer (5), is converted to by board-like ultrasonic transducer (5) to have 42KHZ frequency and 4.2w/cm 2The power ultrasonic of the sound intensity; Conduct radiation in all dust cloud shape metal powder granulates in blending tank is advanced in injection; Cause dither and displacement effect; Stir the dynamic potential energy that forms with mechanical dispersion and match, make metal powder granulates produce displacement, the isostructuralism of colliding, break variation, given play to powerful crystal grain thinning granularity, strengthened the effect of homogeneous dispersion degree.After the ultrasonic wave radiated time reaches 25～28min, close supersonic generator.
---after the ultrasonic wave radiation stops, dispersed with stirring device (4) 3～5min that works on; Treat that dispersed with stirring device (4) stops operation behind the 10min, open discharging opening (13), take out the molybdenum-based rare-earth alloy powder that is mixed and processes.
Shown in accompanying drawing 1, accompanying drawing 3, described low temperature flexibility hydrostatic pressing technology of preparing unit (III) is accomplished by the cryogenic forming mould and the horizontal bidirectional flexible hydraulic harder of original creation design.The cryogenic forming mould is made up of right movable pressing board (20), left movable pressing board (25), pressing plate oriented movable groove (19), cover plate (22), base (23), powder filling die cavity (24) and electrical heating elements; The cryogenic forming mould is fixed on the harder workbench (29), and the right movable pressing board of mould (20) is connected with right oil cylinder pressure head (21), and mould left side movable pressing board (25) is connected with left oil cylinder pressure head (26); Form the closely knit operation unit of dextrad pressure 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 the harder lathe bed (15) through right cylinder bracket (17), be connected with hydraulic operation control cabinet (31) through right oil cylinder oil pipe (16); Form the closely knit operation unit of left-hand pressure 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 the harder lathe bed (15) through left cylinder bracket (27), be connected with hydraulic operation control cabinet (31) through left oil cylinder oil pipe (30).It is other that hydraulic operation control cabinet (31) is fixed on harder lathe bed (15), and 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, manipulation control panel are equipped with in inside.
Low temperature flexibility hydrostatic pressing technology of preparing unit (III), be prepared into the densification of molybdenum-based rare-earth alloy powder pressure have the 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 bigger is:
---according to concrete needs such as the desired density of molybdenum-base rare earth powder metallurgy alloy disk goods, net weight, shape, size; Take into full account factors such as consumption in hydrostatic pressing and sintering type-approval process, scaling loss, shaping porosity, sintering shrinkage, accurately calculate the densification of this batch pressure and be formed in the concrete weight of molybdenum-based rare-earth alloy powder that shaping dies die cavity (24) planted agent loads.
---according to result of calculation, through the electronic-weighing meter of configuration, the molybdenum-based rare-earth alloy powder carried out Weighing after, the interior jolt ramming of cryogenic forming mold cavity (24) of packing into.
---start the electric heating device of cryogenic forming mould, the molybdenum-based rare-earth alloy powder that will be contained in the cryogenic forming mold cavity (24) is heated to 60～70 ℃.
---start horizontal bidirectional flexible hydraulic harder; The static pressure such as bidirectional flexible that rely on hydraulic system the to have function of exerting pressure; Make left and right two oil cylinders (28), (18) can both be with the stable and uniform operating rate of 8mm/min and the powerful flexible working pressure of 300MPa; From pressure and the speed of left and right both direction to be equal to, left and right movable pressing board (25), (20) that stable and uniform ground promotes the cryogenic forming mould apply powerful pliable pressure to the molybdenum-based rare-earth alloy powder that has uniform temperature; Fixed form around the cryogenic forming mould; Under the impressed pressure effect, form the reaction force that equates with this pressure; Around the molybdenum-based rare-earth alloy powder, exert pressure simultaneously; Make molybdenum-based rare-earth alloy powder in the cryogenic forming mold cavity (24) receive simultaneously each to brute force exert pressure, and make each to the pressurized general equilibrium.
---the left and right movable pressing board (25) of cryogenic forming mould, (20) stop to move when being advanced to the gear that is provided with; Left and right oil cylinder (28), (18) are though can not continue to advance at this moment; But still keeping the operational pressure of 300MPa, and continuing to be applied on the molybdenum-based rare-earth alloy powder; Horizontal bidirectional flexible hydraulic harder is after keeping voltage stabilizing 40min under this operational pressure, and take stage by stage unloading pressure means gradually: release speed all-the-time stable is controlled at 6MPa/min; Unload for the first time and be pressed onto 270MPa, voltage stabilizing 10min; Unload for the second time and be pressed onto 210MPa, again voltage stabilizing 5min; Unload for the third time and be pressed onto 120Mpa, again voltage stabilizing 5min; Press the whole pressure of release speed removal of 6MPa/min for the 4th time.
---demoulding, take out the fine and close molybdenum-base rare earth powder metallurgy alloy blank that is shaped of pressure.
Shown in accompanying drawing 1; The described typing of sintering one by one technology of preparing unit (IV); Comprise low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering continuous three sintering works of finalizing the design; Can make the molybdenum-base rare earth powder metallurgy alloy blank shrink great variety such as densification, intensity increase, stable raisings of physical and chemical performance, be prepared into the molybdenum-base rare earth powder metallurgy alloy backing blank process operation technical process that no dirtyization of sizing in surface, the no hierarchical crack in inside, tissue density be evenly distributed and be:
At first carry out the low-temperature bake technical operation:
---the molybdenum-base rare earth powder metallurgy alloy blank is put in the hydrogen atmosphere low-temperature bake stove; Use lower temperature to carry out low-temperature bake; Can make bond strength increase between the molybdenum-based rare-earth alloy particle in the blank, gravitational force between atoms increases on the link surface, makes to take place between alloying pellet to attract bonding to fix; Can eliminate simultaneously the part elasticity internal stress of dissolving blank when pressure is fine and close to be shaped, the most of gas and the moisture content of blank absorption is got rid of in volatilization.The heating rate of low-temperature bake is stable to be controlled at 10 ℃/min (± 2 ℃), and the highest baking temperature is controlled at 480 ℃ (± 5 ℃), all stoving times be controlled at 100min (± 10min), hydrogen flowing quantity is stable in the bake process is controlled at>=0.8m 3/ h.Low-temperature bake cuts off the power supply after reaching stoving time, leans on natural cool-down method cooling in the stove; When treating that temperature is reduced to 120 ℃ in the stove, will toast blank immediately and be transferred to and carry out the intermediate sintering temperature technical operation in the intermediate sintering temperature stove.
Warm presintering technical operation during next carries out:
---the baking blank that will have 120 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate sintering temperature stove that is preheating to equal temperature; Use sufficient temp to carry out intermediate sintering temperature, make to produce big activation energy in the blank, let the atom amplitude of molybdenum-based rare-earth alloy particle strengthen; Abundant atom is entered in the atom graviational interaction scope; Impel multiple migration forms such as atom passes through evaporation, diffusion, flows, cohesion, between the molybdenum-based rare-earth alloy particle, form crystal grain boundary, and progressively move to granule interior; The intergranular reduced distances of molybdenum-based rare-earth alloy, porosity dwindle, density increases thereby make, and finally make the volume contraction of molybdenum-base rare earth powder metallurgy alloy blank; The oxide that can make the molybdenum-based rare-earth alloy particle surface simultaneously is by reduction fully, and the gas of blank absorption, moisture content quilt are all got rid of volatilization, and the internal stress that blank forms in the fine and close shaping of pressure is thoroughly eliminated to be dissolved.The stable 15 ℃/min (± 2 ℃) that is controlled at of the heating rate of intermediate sintering temperature, senior middle school temperature sintering temperature is controlled at 980 ℃ (± 5 ℃), all the intermediate sintering temperature times be controlled at 150min (± 10min) in, hydrogen flowing quantity is stablized and is controlled at>=1.5m in the sintering process 3/ h.Intermediate sintering temperature cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove; When treating that temperature is reduced to 250 ℃ in the stove, the intermediate sintering temperature blank is transferred to carries out the operation of high temperature sintering shaping technology in the intermediate frequency high temperature sintering furnace immediately.
Carry out the operation of high temperature sintering shaping technology at last:
---the intermediate sintering temperature blank that will have 250 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate frequency high temperature sintering furnace that is preheating to equal temperature; Use higher temperature to carry out the high temperature sintering typing of long period; The blank atom diffusion is fully carried out with flowing; 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 typing is divided into 3 stages: from 250 ℃ of temperature, with the heating rate of 15 ℃/min (± 2 ℃) 20min that heats up continuously, make furnace temperature reach 550 ℃, steady temperature 10min; With the programming rate of 10 ℃/min (± 2 ℃) 30min that heats up continuously, make furnace temperature reach 850 ℃, steady temperature 35min again; Be warmed up to 1225 ℃ of the highest controlling values (± 5 ℃) of intermediate frequency high temperature sintering temperature more continuously with the programming rate of 15 ℃/min (± 2 ℃); On this temperature line, steady temperature sintering 120min, make whole sintering times of high temperature intermediate frequency sintering typing be controlled at 240min (± 10min).In the intermediate frequency high temperature sintering type-approval process, hydrogen flowing quantity is stable to be controlled at>=2m 3/ h.The intermediate frequency high temperature sintering cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove; After temperature is reduced to normal temperature in the stove, take out the molybdenum-base rare earth powder metallurgy alloy backing blank of processing.
Shown in accompanying drawing 1; Described classification multi-pass backing technology of preparing unit (V); Comprise horizontal cogging breaking down, vertically roughing, accurate cold rolling three grades of backing operations; Molybdenum-based rare-earth alloy backing blank is all accomplished to the goods form transformation aspect many at interior tissue, geometry, mechanical and physical performance etc., be prepared into and be convenient to meticulous in-depth and be processed into the molybdenum-base rare earth powder metallurgy sheet alloy process operation technical process of orienting articles and be:
At first carry out the horizontal cogging breaking down of multi-pass technical operation:
---put molybdenum-base rare earth powder metallurgy alloy backing blank in the hydrogen atmosphere heating furnace of configuration into, carry out the first fire heating; 1200～1300 ℃ of heating-up temperatures, heat time heating time 80～90min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls, carried 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%.
---accomplish the first fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere heating furnace again, carry out the second fire heating; 1100～1200 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls again, still used≤mill speed of 30m/min, carry out taking turns 3 passage lateral shuttle cogging breaking down operations more continuously; Average every time working modulus>=20%.
---accomplish the 2nd fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere annealing furnace, the heat retaining operation of annealing is handled; 850～870 ℃ of annealing temperatures, annealing high temperature retention time 30～40min, hydrogen flowing quantity >=0.5m3/h.Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply; The backing blank is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace.
Next carries out the vertical roughing technical operation of multi-pass:
---the backing blank that will pass through the cogging breaking down is put in the hydrogen atmosphere heating furnace, carries out the first fire heating; 950～1050 ℃ of heating-up temperatures, heat time heating time 70～80min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, vertically put the backing blank on the four roller reversibly hot milling trains immediately, carry out continuous 3 passages and vertically come and go the roughing operation; Hot mill rolling power>=400t, roll specification Φ 180 * 400mm, mill speed≤45m/min, on average every time working modulus≤12%.
---accomplish the first fiery heating rolling after, put the backing blank again in the hydrogen atmosphere heating furnace immediately, carry out the 2nd fire heating; 900～1000 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h.After completion adds hot work, put the backing blank again on the four roller reversible hot milling rolls immediately, still use≤mill speed of 45m/min, carry out taking turns 3 passages more continuously and vertically come and go the roughing operation, on average every time working modulus≤10% is rolled into the backing plate.
---accomplish the 2nd fiery heating rolling after, immediately the backing plate is put in the hydrogen atmosphere annealing furnace, the heat retaining operation of annealing is handled; 850～870 ℃ of annealing temperatures, annealing high temperature retention time 50～60min, hydrogen flowing quantity>=0.5m 3/ h.Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply; The backing plate is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace.
---will accomplish vertical roughing and the cooled backing plate of annealing; Deliver on the plate shearing machine, tentatively cut the limit correction of the flank shape, excise the surplus limit of irregular calendering; Can reduce accurate cold rolling power consumption, in time reclaim the tailing utilization of molybdenum-based rare-earth alloy backing plate.
Carry out the accurate cold rolling technical operation of multi-pass at last:
---thoroughly clear up carrying out accurate cold rolling backing panel surface, hard foreign material such as the burr of avoiding adhering to, decortication cause impression, draw mass defects such as mark panel surface.After accomplishing prune job, smear very thin one deck cold-rolling lubricant in panel surface with cotton yarn.
---the plate that will pass through removing surface is vertically put on the reversible precise cold milling train of four rollers, carries out the first time continuous 3 passages and vertically comes and goes accurate cold rolling; 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 accomplish the plate of the 1st precision after cold rolling, carry out again thoroughly cleaning of surface; Smear cold-rolling lubricant with cotton yarn in panel surface once more.
---will vertically put into once more on the reversible precise cold milling train of four rollers through the plate of the 2nd subsurface cleaning, still with the mill speed of≤60m/min, carry out continuously again 3 passages vertically come and go accurate cold rolling, average every time working modulus≤2%; The molybdenum-base rare earth powder metallurgy sheet alloy is processed in final backing, and reaches the gauge tolerance standard of technical papers regulation.
Shown in accompanying drawing 1; Technology of preparing unit (VI) is processed in described retrofit; Comprise stamping-out shaping, elementary grinding, the continuous three kinds of fine processing methods of fine gtinding, can the molybdenum-base rare earth powder metallurgy sheet alloy that backing is processed be prepared into and use the user the directly directed molybdenum-base rare earth powder metallurgy alloy disk goods process operation technical process that uses to be:
---sheet material is put on the hydraulic plate shears,, used pliable pressure to be cut into the bar shaped plate by the molybdenum-base rare earth powder metallurgy alloy disk goods specification that uses customer requirements; The hydraulic plate shears of configuration cut out thickness 0.8～4.0mm, cut out length >=1000mm.
---the bar shaped plate is put on the hydraulic press,, pressed the specification tolerance of molybdenum-base rare earth powder metallurgy alloy disk goods, use the circular sheet stock of pliable pressure stamping-out through disk hydraulic pressure blanking die; Stamping-out pressure >=the 100t of the hydraulic press of configuration towards circular diameter Φ 25～110mm, dashes circle thickness 0.8～4.0mm.
---circular sheet stock put into carry out elementary attrition process on the disk grinder; Use common cooling fluid during elementary grinding, allowance 0.06～0.08mm, lap speed is selected 800～1000r/min.
---the circular sheet stock that will pass through elementary grinding is put on the disc type precision lapping machine, finally processes fine gtinding processing; Fine gtinding adds man-hour, and grinding agent selects to use W20 schmigel+20 #Machine oil (proportioning 1: 15～20), lap speed is selected 1500～2000r/min.
Shown in accompanying drawing 1; Described commodity finishing and packing technology of preparing unit (VII) is the technical standard requirement of dispatching from the factory according to molybdenum-base rare earth powder metallurgy alloy disk goods, carries out clean and tidy, commercializations processing such as cleaning is anticorrosion, sign, anticollision packing; After fulfiling assignment, pin is treated in the warehouse-in keeping.

Claims (7)

1. molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof; It is characterized in that: this molybdenum-base rare earth powder metallurgy alloy disk and preparation method thereof comprises that polynary group of material proportioning (I), ultrasonic homogeneous are mixed (II), low temperature flexibility hydrostatic pressing (III), the technical equipment of (VI), commodity finishing and packing (VII) technology of preparing unit and configuration thereof, the technical parameter of execution are processed in sintering typing (IV), classification multi-pass backing (V), retrofit one by one.
2. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof; It is characterized in that: described polynary group of material proportioning technology of preparing unit (I); The molybdenum-base rare earth powder metallurgy alloy disk group material component proportioning share that adopts; Batch to manufacture a molybdenum-base rare earth powder metallurgy alloy disk goods gross weight is radix, the proportioning share of various batching components by weight: pure molybdenum powder (M 0) [93.0～95.0] part; Lanthana (La 2O 3) [2.2～2.5] part; Cerium oxide (Ce 2O 3) [1.6～2.0] part; Neodymia (NdO 2) [1.2～1.5] part.
3. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof is characterized in that: the described ultrasonic homogeneous technology of preparing unit (II) that is mixed, accomplish by the ultrasonic homogeneous compounder of the metal dust of configuration; The ultrasonic homogeneous compounder of metal dust, global design are helped sealing circular cone jar type structure of container, are 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 through 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) through total terminal box (3), bundle conductor (2);
Board-like ultrasonic transducer (5) installs and fixes with hexagonal angle branch position along blending tank tank body (11) outer wall; Metal dust atomization charger (7); Form by metal dust holding vessel, high-pressure spray pump, powder jet; Be fixed on the blending tank cover (9) with branch position, 60 ° of angles of concentric circles; 3 pure molybdenum powders that the equivalent of packing into is divided equally wherein, all the other 3 are respectively charged into 3 kinds of RE oxide powders, and distribution is put in 4 kinds of metal dusts submission displacements; Dispersed with stirring device (4); Be fixed on blending tank cover (9) center; Select frequency control motor as driving power source; On shaft, be mounted with 2 groups and go to upper and lower double-deck the layout, each group all has 2 reverse hock type dispersed with stirring dishes of installing, and the periphery of each dispersion impeller all is mounted with some hocks;
Ultrasonic homogeneous is mixed technology of preparing unit (II) batching component elemental metals powder, and the solid phase homogeneous is mixed and is prepared into that constituent element is evenly distributed, the preparation technology's job step and the technical parameter of the molybdenum-based rare-earth alloy powder of loose particles standard are:
---according to the group material ratio requirement of claim 2 regulation, press the filling rate of the ultrasonic homogeneous compounder of metal powder dischargeable capacity 58%, calculate the concrete weight that batching component elemental metals powder feeds intake;
---according to result of calculation, through the electronic-weighing meter of configuration, batching component elemental metals powder carried out Weighing after, be respectively charged in the corresponding metal dust atomization charger (7);
---start vacuum air pump (6), extract the air in the 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 3The time, close the gas injection pump;
---start 6 metal dust atomization chargers (7) immediately simultaneously, 4 kinds of elemental metals powder of batching component with the dust cloud shape simultaneously continuous injection advance in the blending tank, all spray the material time to be controlled in 18～20min and to accomplish;
---meanwhile; Start dispersed with stirring device (4); Drive all dust cloud shape metal powder granulates that spray in the blending tank with the rotating speed of 1200r/min and flow fast with the two-way route that stirs continuously, realize to group material component elemental metals powder homogeneous dispersion, mix operation;
---meanwhile, the supersonic generator in the startup automaton (1) arrives ultrasonic couple electrical energy on the board-like ultrasonic transducer (5), is converted to by board-like ultrasonic transducer (5) to have 42KHZ frequency and 4.2w/cm 2The power ultrasonic of the sound intensity, conduct radiation in all the dust cloud shape metal powder granulates in blending tank is advanced in injection after the ultrasonic wave radiated time reaches 25～28min, is closed supersonic generator;
---after the ultrasonic wave radiation stopped, dispersed with stirring device (4) 3～5min that works on treated that dispersed with stirring device (4) stops operation behind the 10min, opens discharging opening (13) and takes out the molybdenum-based rare-earth alloy powder that is mixed and processes.
4. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof; It is characterized in that: described low temperature flexibility hydrostatic pressing technology of preparing unit (III), accomplish by the cryogenic forming mould and the horizontal bidirectional flexible hydraulic harder of configuration; The cryogenic forming mould is made up of right movable pressing board (20), left movable pressing board (25), pressing plate oriented movable groove (19), cover plate (22), base (23), powder filling die cavity (24) and electrical heating elements; The cryogenic forming mould is fixed on the harder workbench (29), and the right movable pressing board of mould (20) is connected with right oil cylinder pressure head (21), and mould left side movable pressing board (25) is connected with left oil cylinder pressure head (26); Form the closely knit operation unit of dextrad pressure 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 the harder lathe bed (15) through right cylinder bracket (17), be connected with hydraulic operation control cabinet (31) through right oil cylinder oil pipe (16); Form the closely knit operation unit of left-hand pressure 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 the harder lathe bed (15) through left cylinder bracket (27), be connected with hydraulic operation control cabinet (31) through left oil cylinder oil pipe (30); It is other that hydraulic operation control cabinet (31) is fixed on harder lathe bed (15), and 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, manipulation control panel are equipped with in inside;
Low temperature flexibility hydrostatic pressing technology of preparing unit (III) is the molybdenum-based rare-earth alloy powder, the pressure densification be prepared into have the definite shape size, pressurized general equilibrium, Density Distribution evenly, the preparation technology's job step and the technical parameter of molybdenum-base rare earth powder metallurgy alloy blank that structural strength is bigger be:
---according to density, net weight, shape, the dimensional requirement of molybdenum-base rare earth powder metallurgy alloy disk goods; Take into full account consumption, scaling loss factor in hydrostatic pressing and sintering type-approval process, calculate the fine and close shaping of batch pressure should be loaded the molybdenum-based rare-earth alloy powder in shaping dies die cavity (24) concrete weight;
---according to result of calculation, through the electronic-weighing meter of configuration, the molybdenum-based rare-earth alloy powder carried out Weighing after, the interior jolt ramming of cryogenic forming mold cavity (24) of packing into;
---start the electric heating device of cryogenic forming mould, the molybdenum-based rare-earth alloy powder that will be seated in the cryogenic forming mold cavity (24) is heated to 60～70 ℃;
---start horizontal bidirectional flexible hydraulic harder; Make left and right two oil cylinders (28), (18) all with the stable and uniform operating rate of 8mm/min and the powerful flexible working pressure of 300MPa; From pressure and the speed of left and right both direction to be equal to; Left and right movable pressing board (25), (20) that stable and uniform ground promotes the cryogenic forming mould apply powerful pliable pressure to the molybdenum-based rare-earth alloy powder that has uniform temperature;
---the left and right movable pressing board (25) of cryogenic forming mould, (20) stop to move when being advanced to the gear that is provided with; Left and right oil cylinder (28), (18) are though can not continue to advance at this moment; But still keeping the operational pressure of 300MPa, and continuing to be applied on the molybdenum-based rare-earth alloy powder; Horizontal bidirectional flexible hydraulic harder is after keeping voltage stabilizing 40min under this operational pressure, and take stage by stage unloading pressure means gradually: release speed all-the-time stable is controlled at 6MPa/min; Unload for the first time and be pressed onto 270MPa, voltage stabilizing 10min; Unload for the second time and be pressed onto 210MPa, again voltage stabilizing 5min; Unload for the third time and be pressed onto 120Mpa, again voltage stabilizing 5min; Press the whole pressure of release speed removal of 6MPa/min for the 4th time;
---demoulding, take out the fine and close molybdenum-base rare earth powder metallurgy alloy blank that is shaped of pressure.
5. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof; It is characterized in that: the described typing of sintering one by one technology of preparing unit (IV); Comprise low-temperature bake, middle temperature presintering, intermediate frequency high temperature sintering continuous three sintering works of finalizing the design, accomplish by hydrogen atmosphere low-temperature bake stove, hydrogen atmosphere intermediate sintering temperature stove, the hydrogen atmosphere intermediate frequency high temperature sintering furnace of configuration; With the molybdenum-base rare earth powder metallurgy alloy blank one by one the sintering preparation technology's job step and the technical parameter that are fixed to the molybdenum-base rare earth powder metallurgy alloy backing blank that no dirtyization of sizing in surface, inside no hierarchical crack, tissue density be evenly distributed be:
At first, carry out the low-temperature bake technical operation:
---the molybdenum-base rare earth powder metallurgy alloy blank is put in the hydrogen atmosphere low-temperature bake stove; Use lower temperature to carry out low-temperature bake; The stable 10 ℃/min (± 2 ℃) that is controlled at of the heating rate of baking; The highest baking temperature is controlled at 480 ℃ (± 5 ℃), all stoving times be controlled at 100min (± 10min), hydrogen flowing quantity is stable in the bake process is controlled at>=0.8m 3/ h; Low-temperature bake cuts off the power supply after reaching stoving time, leans on natural cool-down method cooling in the stove, when treating that temperature is reduced to 120 ℃ in the stove, the low-temperature bake blank is transferred to carries out the intermediate sintering temperature technical operation in the intermediate sintering temperature stove immediately;
Secondly, warm presintering technical operation in carrying out:
---the baking blank that will have 120 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate sintering temperature stove that is preheating to equal temperature; Use sufficient temp to carry out intermediate sintering temperature; The stable 15 ℃/min (± 2 ℃) that is controlled at of the heating rate of sintering; Senior middle school temperature sintering temperature is controlled at 980 ℃ (± 5 ℃), all the intermediate sintering temperature times be controlled at 150min (± 10min) in, hydrogen flowing quantity is stable in the sintering process is controlled at>=1.5m 3/ h; Intermediate sintering temperature cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove, when treating that temperature is reduced to 250 ℃ in the stove, the intermediate sintering temperature blank is transferred to carries out the operation of high temperature sintering shaping technology in the intermediate frequency high temperature sintering furnace immediately;
At last, carry out the operation of high temperature sintering shaping technology:
---the intermediate sintering temperature blank that will have 250 ℃ of surplus temperature is put in the hydrogen atmosphere intermediate frequency high temperature sintering furnace that is preheating to equal temperature; Use higher temperature to carry out the high temperature sintering typing of long period; The heating rate of sintering typing is divided into 3 stages: from 250 ℃ of temperature; With the heating rate of 15 ℃/min (± 2 ℃) 20min that heats up continuously, make furnace temperature reach 550 ℃, steady temperature 10min; With the programming rate of 10 ℃/min (± 2 ℃) 30min that heats up continuously, make furnace temperature reach 850 ℃, steady temperature 35min again; Programming rate with 15 ℃/min (± 2 ℃) is warmed up to 1225 ℃ of the highest controlling values (± 5 ℃) continuously again; On this temperature line, steady temperature sintering 120min, make whole sintering times be controlled at 240min (± 10min); In the intermediate frequency high temperature sintering type-approval process, hydrogen flowing quantity is stable to be controlled at>=2m 3/ h; The intermediate frequency high temperature sintering cuts off the power supply after reaching sintering time, leans on natural cool-down method cooling in the stove, treat that temperature is reduced to normal temperature in the stove after, take out the molybdenum-base rare earth powder metallurgy alloy backing blank of processing.
6. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof; It is characterized in that: described classification multi-pass backing technology of preparing unit (V); Comprise horizontal cogging breaking down, vertically roughing, accurate cold rolling continuous three grades of backing operations, accomplish by hydrogen atmosphere heating furnace, hydrogen atmosphere annealing furnace, four roller reversible hot milling rolls, the reversible precise cold milling train of four rollers, the plate shearing machine of configuration; Molybdenum-base rare earth powder metallurgy alloy backing blank classification backing is become to be suitable for preparation technology's job step and technical parameter that meticulous in-depth is processed as the molybdenum-base rare earth powder metallurgy sheet alloy of orienting articles is:
At first, carry out the horizontal cogging breaking down of multi-pass technical operation:
---put molybdenum-base rare earth powder metallurgy alloy backing blank in the hydrogen atmosphere heating furnace of configuration into, carry out the first fire heating, 1200～1300 ℃ of heating-up temperatures, heat time heating time 80～90min, hydrogen flowing quantity>=0.8m 3/ h; After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls, carried 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%;
---accomplish the first fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere heating furnace again, carry out the second fire heating, 1100～1200 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h; After completion adds hot work, immediately the backing blank is laterally put in the four roller reversible hot milling rolls again, still used≤mill speed of 30m/min, carry out taking turns 3 passage lateral shuttle cogging breaking down operation, on average every time working modulus>=20% more continuously;
---accomplish the 2nd fiery heating rolling after, immediately the backing blank is put in the hydrogen atmosphere annealing furnace, the heat retaining operation of annealing is handled, 850～870 ℃ of annealing temperatures, annealing high temperature retention time 30～40min, hydrogen flowing quantity >=0.5m3/h; Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply, the backing blank is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace;
Secondly, carry out the vertical roughing technical operation of multi-pass:
---the backing blank that will pass through the cogging breaking down is put in the hydrogen atmosphere heating furnace, carries out the first fire heating, 950～1050 ℃ of heating-up temperatures, heat time heating time 70～80min, hydrogen flowing quantity>=0.8m 3/ h; After completion adds hot work, vertically put the backing blank on the four roller reversible hot milling rolls immediately, carry out continuous 3 passages and vertically come and go the roughing operation; Hot mill rolling power>=400t; Roll specification Φ 180 * 400mm, mill speed≤45m/min, on average every time working modulus≤12%;
---accomplish the first fiery heating rolling after, put the backing blank again in the hydrogen atmosphere heating furnace immediately, carry out the 2nd fire heating, 900～1000 ℃ of heating-up temperatures, heat time heating time 40～50min, hydrogen flowing quantity>=0.8m 3/ h; After completion adds hot work, put the backing blank again on the four roller reversible hot milling rolls immediately, still use≤mill speed of 45m/min, carry out taking turns 3 passages more continuously and vertically come and go the roughing operation, on average every time working modulus≤10% is rolled into the backing plate;
---accomplish the 2nd fiery heating rolling after, immediately the backing plate is put in the hydrogen atmosphere annealing furnace, the operation of annealing is handled, 850～870 ℃ of annealing temperatures, annealing high temperature retention time 50～60min, hydrogen flowing quantity>=0.5m 3/ h; Cut off the power supply after reaching the annealing temperature retention time, stop hydrogen supply, the backing plate is cooling cooling back taking-up naturally in the hydrogen atmosphere annealing furnace;
---will accomplish vertical roughing and the cooled backing plate of annealing; Deliver on the plate shearing machine, tentatively cut the limit correction of the flank shape, excise the surplus limit of irregular calendering; Can reduce accurate cold rolling power consumption, in time reclaim the tailing utilization of molybdenum-based rare-earth alloy backing plate;
At last, carry out the accurate cold rolling technical operation of multi-pass:
---thoroughly clear up carrying out accurate cold rolling backing panel surface, hard foreign material such as the burr of avoiding adhering to, decortication cause impression, draw mass defects such as mark panel surface; After accomplishing prune job, smear very thin one deck cold-rolling lubricant in panel surface with cotton yarn;
---the plate that will pass through removing surface is vertically put on the reversible precise cold milling train of four rollers; It is cold rolling to carry out the vertically round precision of the continuous 3 passages first time, the roll-force>=400t of precise cold milling train, roll specification Φ 180 * 400mm; Mill speed≤60m/min, on average every time working modulus≤5%;
---will accomplish the plate of the 1st precision after cold rolling, carry out again thoroughly cleaning of surface, smear cold-rolling lubricant with cotton yarn in panel surface once more;
---will vertically put into once more on the reversible precise cold milling train of four rollers through the plate of the 2nd subsurface cleaning; Still with the mill speed of≤60m/min; Carrying out 3 passages more continuously vertically comes and goes accurate cold rolling; Average every time working modulus≤2%, the molybdenum-base rare earth powder metallurgy sheet alloy is processed in final backing, and reaches the gauge tolerance standard of technical papers regulation.
7. a kind of molybdenum-base rare earth powder metallurgy alloy disk according to claim 1 and preparation method thereof; It is characterized in that: technology of preparing unit (VI) is processed in described retrofit; Comprise stamping-out shaping, elementary grinding, the continuous fine processing method of fine gtinding, accomplish by hydraulic plate shears, hydraulic press, disk grinder, the disc type precision lapping machine of configuration; With the retrofit of molybdenum-base rare earth powder metallurgy sheet alloy become to use the user directly the preparation technology's job step and the technical parameter of the molybdenum-base rare earth powder metallurgy alloy disk goods of directed use be:
---the molybdenum-base rare earth powder metallurgy sheet alloy is put on the hydraulic plate shears,, used pliable pressure to be cut into the bar shaped plate by the molybdenum-base rare earth powder metallurgy alloy disk goods specification that uses customer requirements; The hydraulic plate shears of configuration cut out thickness 0.8～4.0mm, cut out length >=1000mm;
---the bar shaped plate is put on the hydraulic press,,, used the circular sheet stock of pliable pressure stamping-out by the molybdenum-base rare earth powder metallurgy alloy disk goods specification tolerance that uses customer requirements through disk hydraulic pressure blanking die; Stamping-out pressure >=the 100t of the hydraulic press of configuration towards circular diameter Φ 25～110mm, dashes circle thickness 0.8～4.0mm;
---circular sheet stock put into carry out elementary attrition process on the disk grinder, use common cooling fluid during elementary grinding, allowance 0.06～0.08mm, lap speed is selected 800～1000r/min;
---the circular sheet stock that will pass through elementary grinding is put on the disc type precision lapping machine, finally processes fine gtinding processing; Fine gtinding adds man-hour, and grinding agent selects to use W20 schmigel+20 #Machine oil (proportioning 1: 15～20), lap speed is selected 1500～2000r/min, processes molybdenum-base rare earth powder metallurgy alloy disk goods at last.
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CN109940158A (en) * 2019-04-03 2019-06-28 中南大学 A kind of quick preparation process of fine grain molybdenum plate
CN109940158B (en) * 2019-04-03 2020-05-12 中南大学 Rapid preparation process of fine-grain molybdenum plate
CN113976887A (en) * 2021-11-09 2022-01-28 武渝钦 Pressurization type molybdenum powder sintering box suitable for rare earth preparation
CN115041685A (en) * 2022-05-25 2022-09-13 邯郸新兴特种管材有限公司 Method for forming molybdenum tube

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