CN101423911B - Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof - Google Patents
Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof Download PDFInfo
- Publication number
- CN101423911B CN101423911B CN2007100562583A CN200710056258A CN101423911B CN 101423911 B CN101423911 B CN 101423911B CN 2007100562583 A CN2007100562583 A CN 2007100562583A CN 200710056258 A CN200710056258 A CN 200710056258A CN 101423911 B CN101423911 B CN 101423911B
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- earth alloy
- rolling
- based rare
- sintering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Powder Metallurgy (AREA)
Abstract
The invention relates to a process for manufacturing the molybdenum based rare earth alloy plate and equipment for manufacturing the same, wherein pure molybdenum powder is simultaneously added with four rare earth oxides of ZrO2, Y2O3, La2O3 and Nd2O3 according to certain ratio, by utilizing the chrematistics of long and large crystal grain and strong sag resistance and anti-creep property of rare earth alloy elements and the dispersion strengthening function, the re-crystallization temperature of the metal molybdenum is increased, the mechanical performances of the molybdenum based material such as tensile property, yielding behavior and extensibility are improved, and the application range of the molybdenum based material is widened; and the manufacturing process comprises production procedures of material preparation treatment, mixing treatment, forming treatment, sintering treatment, material making treatment and the like and the setting of various technical parameters of special technical equipment and process. With the preparation process, the molybdenum based rare earth alloy plate which has the advantages of good electric conductivity and heat conductivity, excellent high-temperature resistance and corrosion resistance and better mechanical performances such as tensile property, yielding behavior and extensibility, and fills in domestic blank and can replace the imported material can be manufactured.
Description
Technical field
The present invention relates to a kind of manufacturing process and equipment thereof of sheet alloy, specifically a kind of manufacturing process of molybdenum-based rare-earth alloy slab and equipment thereof.
Background technology
Molybdenum substrate material is because of its distinctive high-melting-point, good electrical conductivity, thermal conductivity, and superior erosion resistance, anti-ray ability are widely used in the production industries such as electronics, electric power, space flight, automobile, metallurgy.Along with improving constantly of China's scientific and technological level, each production field high-tech product continues to bring out, the Application Areas of molybdenum substrate material is expanded day by day, and the demand usage quantity sharply increases, and requires also more and more higher to material property, tolerance of dimension, surface quality, manufacturing cost etc. simultaneously.But, because the recrystallization temperature of molybdenum is low, and very easily brittle failure behind the recrystallize, processing difficulties, saw lumber is difficult for, and has seriously restricted the production development of molybdenum substrate material; Only doing support with the molybdenum substrate material manufacturing technology and the corresponding specific equipment of advanced science, just can provide large batch of high-quality molybdenum substrate material and goods thereof, could be national economy and national defense construction service better.
The research and development production of molybdenum in China substrate material is started in the eighties mid-term in last century, development is faster just arranged after entering 21st century.But no matter the process for processing state of the art of the existing molybdenum substrate material of China is Technology or capacity of equipment, no matter is product performance or breed structure, all with world industrially-advanced country big gap is arranged; Particularly be wanting in apart from bigger in the preparation of high-quality slab, sintering temperature control, rolling equipment ability, operation of rolling control, stocking surface quality, sheet material specification kind etc., the needs that can not adapt to the Chinese national economy high speed development far away cause a large amount of imports of having to of a lot of molybdenum substrate materials.
The enterprise that present China is engaged in molybdenum base alloy sheet material research and development production is a lot, but the enterprise with complete process route and complete production process equipment facility seldom, because of being subjected to the restriction of molybdenum base alloy sheet material industry overall technology level, above-mentioned enterprise exists the obvious gap of alloy proportion reasonableness, blank homogeneous purifying, sintering process arrangement and the aspects such as temperature control, rolling technology arrangement, board quality and specification kind of molybdenum substrate material.
Summary of the invention
The objective of the invention is to solve weakness or the deficiency that domestic existing molybdenum base alloy sheet material exists at the aspects such as batching, blending equipment, forming technology and facility, sintering process arrangement, rolled plate processing method of mixing, a kind of manufacturing process with molybdenum-based rare-earth alloy slab of good mechanical properties is provided, a kind of specific equipment that can satisfy advanced technologies parameter and processing requirement is provided simultaneously.
Purpose of the present invention is achieved by the following technical programs:
Molybdenum-based rare-earth alloy slab of the present invention is by mix ZrO simultaneously in pure molybdenum powder
2, Y
2O
3, La
2O
3, Nd
2O
3Four kinds of rare earth oxide manufacturings form, and its each proportion of raw materials is: 100 parts of pure molybdenum powders, ZrO
20.5 part, Y
2O
32 parts, La
2O
3: 2.5 parts, Nd
2O
3: 1 part.
Molybdenum-based rare-earth alloy slab of the present invention is handled five manufacturing technology steps by batching processing, combination treatment, shaping processing, sintering processes, saw lumber and is finished realization.
Concrete manufacturing process is as follows:
1, batching is handled: this treating processes is to carry out the based process process that group element material is prepared for manufacturing molybdenum-based rare-earth alloy slab.Proportionally choose raw material, pure molybdenum powder, ZrO
2, Y
2O
3, La
2O
3, Nd
2O
3According to mixing the rare earth oxide characteristics, adopt the distilled water method of sizing mixing, whole rare earth oxides according to Weighing add up to 2.8 times of gross weight to be equipped with distilled water, the whole rare earth oxides of dissolving in the heated and stirred dissolving vessel, and then filter by hay tank, remove impurity, make the lysate that contains four kinds of rare earth oxides.
2, combination treatment: this treating processes is to handle for molybdenum-based rare-earth alloy slab is shaped, and prepares a kind of processes manufacturing processed of molybdenum-based rare-earth alloy powder.Described combination treatment process is to mix 4 kinds of rare earth oxide lysates by the even spray of spiral spray mixing tank in pure molybdenum powder, and then with the material after the blending through horizontal vibration drying sieve dry, pulverizing, Screening Treatment, purpose is all group material of forming the molybdenum-based rare-earth alloy powder, be uniformly mixed into that globule size is unified, constituent element is evenly distributed, do wet appropriateness, the high-quality shaping raw material powder of loose nothing caking, the molybdenum-based rare-earth alloy powder of making after combination treatment processing should be contained in temporary for some time in the stainless steel cylinder; But the temporary time should be above 24 hours.
3, shaping is handled: this treating processes is the molybdenum-based rare-earth alloy powder that will be mixed and made into, and a kind of technology that closely knit one-tenth has the blank of definite shape, size, porosity, intensity adds treating processes.The main technique content is at first according to consume factors such as the scaling loss in finished product parameters such as the density of molybdenum-based rare-earth alloy slab, thickness, planar dimension and sintering, the saw lumber course of processing, edgings, calculate required molybdenum-based rare-earth alloy powder weight after, weigh and get the raw materials ready; And then dimensional parameters and the shaping factors such as reservation porosity (general plate shape base material porosity select 40%), density required according to the shaping blank, adjust length and width, the thick dimensional parameters of setting plate shape blank mold; Adorn mould at last, the molybdenum-based rare-earth alloy powder compression that will be mixed and made into by the hydraulic bidirectional harder become pressurized general equilibrium, density distribution evenly, molybdenum-based rare-earth alloy slab blank that structural strength is bigger.
4, sintering processes: this treating processes is after the molybdenum-based rare-earth alloy slab blank body is heated in suitable atmosphere and temperature, shrinks a kind of technological process of densification, intensity increase, physical and chemical performance raising steady change.The main technique content is the molybdenum-based rare-earth alloy slab blank body of press forming, sinters no dirtyization of sizing in surface, the no hierarchical crack in inside into, the molybdenum-based rare-earth alloy slab goods base material of suitable density, intensity and physics of metals characteristic is arranged.
1., initial stage of sintering processes process, adopt the hydrogen atmosphere roaster in hydrogen atmosphere, to use lesser temps to toast, the bond strength between metallic particles is increased, interatomic gravitation increase bonds between particle on the link surface.This bonding has the character of Van der Waals force, do not need the particle atom to do obvious displacement, have only the arrangement change or the position adjustment of part of atoms, though blank body does not have obvious contraction, density is also constant substantially, but the intravital elasticity internal stress of blank is eliminated, also can volatilizees and get rid of the gas and the moisture content of blank body absorption, decomposition-reduction partial oxide.
2., mid-term of sintering processes process, adopt hydrogen atmosphere pre-burning freezing of a furnace in hydrogen atmosphere, to use sufficient temp to carry out presintering, form big intensity of activation, allow the amplitude increasing of atomic vibration, make abundant atom enter atom reactive force scope; Impel migration forms such as atom passes through evaporation, diffusion, flows, cohesion, form crystal grain boundary at granular boundary, and crystal grain boundary is moved to granule interior, and cause grain growth or move making crystal grain merge (that is: recrystallize) by crystal boundary, produce volume diffusion, surface diffusion and crystal boundary diffusion.Design arranges the result of this presintering to be: grain spacing is from shortening, porosity dwindles, density increases, blank body is shunk through sintering, and the oxide compound of particle surface is reduced fully, the gas of blank body absorption, moisture content and impurity quilt are all got rid of volatilization, and the internal stress that particle surface contact connection forms in the blank body pressed compact process is also thoroughly cleared up.
3., the later stage of sintering processes process, in hydrogen atmosphere, use comparatively high temps and longer soaking time in the horizontal intermediate frequency sintering oven of hydrogen atmosphere, to carry out last sintering, make the atomic diffusion of blank body and move to flow and obtain more abundant carrying out, hole quantity and size are fully reduced, and established good physical, chemistry, mechanical property obtain fully stable.
The sintering processes processes manufacturing technology of the present invention's design, be the sintering process method of taking to be divided into three different stepss such as baking, presintering, intermediate frequency sintering, realize by the technical data of configuration " hydrogen atmosphere roaster ", " hydrogen atmosphere pre-burning freezing of a furnace " and general agglomerating plants such as " the horizontal intermediate frequency sintering ovens of hydrogen atmosphere " and unique design.
The present invention is according to above-mentioned densified sintering product mechanism and test of many times, contrast preference data, and the sintering processes processes technical parameter of design is:
Baking process parameter: baking top temperature: 700 ℃
Temperature rise rate: 10 ℃/min
Storing time: 240min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 0.8m
3/ h
Pre-sintering process parameter: presintering top temperature: 1050 ℃
Temperature rise rate: 20 ℃/min
Sintering time: 260min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 1.5m
3/ h
Intermediate frequency sintering process parameter: intermediate frequency sintering top temperature: 1850 ℃
Temperature rise rate: 15 ℃/min * 50min
10℃/min×40min
15℃/min×45min
Sintering time: 360min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 2m
3/ h
5, saw lumber is handled: this treating processes is molybdenum-based rare-earth alloy slab goods base material, finishes a kind of processes manufacturing processed that turns to geometrical shape, weave construction, mechanical property, the processing performance of goods attitude to change from sintered state.The main technique content is the molybdenum-based rare-earth alloy slab goods base material of finishing sintering processes, and processing and manufacturing becomes can be directly used in a kind of molybdenum-based rare-earth alloy slab kind of production industries such as electronics, electric power, space flight, automobile, metallurgy.
Described saw lumber treating processes is to take the cogging breaking down, intersect warm-rolling, three grades of segmentation rolling technology methods such as accurate cold rolling; And the special technology of technique processing method, technical data and configuration by unique design in every section operation of rolling is equipped and is realized.Cogging breaking down that design is arranged, intersect warm-rolling, accurate cold rolling etc. three grades rolling in, all designed Heating temperature, heat-up time, a heating rolling passage respectively, the technique processing method and the technical data of original creation such as pass reduction, rolling direction, annealing temperature, annealing time:
Cogging breaking down: first fire: Heating temperature: 1150～1300 ℃
Heat-up time: 80～90min
Fire time rolling pass: 3 times
Pass reduction :≤20%
Rolling direction: whole transverse rollings
Second fire: Heating temperature: 1100～1200 ℃
Heat-up time: 40～50min
Fire time rolling pass: 3 times
Pass reduction :≤15%
Rolling direction: whole transverse rollings
Anneal: annealing temperature: 900 ℃ ± 10 ℃
Annealing soaking time: 〉=40min
Intersection warm-rolling: first fire: Heating temperature: 950～1050 ℃
Heat-up time: 70～80min
Fire time rolling pass: 3 times
Pass reduction :≤12%
Rolling direction: vertically, laterally, vertically tandem rolling again
Second fire: Heating temperature: 850～950 ℃
Heat-up time: 40～50min
Fire time rolling pass: 3 times
Pass reduction :≤10%
Rolling direction: vertically, laterally, vertically tandem rolling again
Anneal: annealing temperature: 900 ℃ ± 10 ℃
Annealing soaking time: 〉=60min
Accurate cold rolling: finish rolling for the first time: last pass: 3 times
Pass reduction :≤5%
Rolling direction: all vertically rolling
Finish rolling for the second time: last pass: 2 times
Pass reduction :≤2%
Rolling direction: all vertically rolling
Described saw lumber treatment process process need be passed through alkali cleaning again after annealed operation, alkaline wash is selected the KOH of proportioning 30% for use, and the alkaline wash temperature is controlled at 80 ℃～90 ℃.
Described saw lumber treatment process process also needs by adding cold-rolling lubricant and polished finish being carried out on the cold rolled sheet surface, and this finishing rolling technology method can effectively improve the surface quality rank of molybdenum-based rare-earth alloy slab, enlarges use range.
Specific equipment spiral spray mixing tank in the described combination treatment process comprises the auger motor, auger, pure molybdenum powder charging opening, spray header, rare earth oxide lysate hold tank, the high-pressure spraying pump, the double spiral agitator motor, the compound import, double spiral agitator, the compound outlet, body A, B, the auger that a described end is connected with the auger motor is arranged on the inside of body A, the double spiral agitator that one end is connected with the double spiral agitator motor is arranged on the inside of body B, body A and body B are communicated with by the compound import, rare earth oxide lysate hold tank and high-pressure spraying pump be arranged on body A above, on body A, have pure molybdenum powder charging opening, have spray header below the rare earth oxide lysate hold tank, on body B, have the compound outlet.
Working process is: will add in the bed piece by pure molybdenum powder charging opening through the pure molybdenum powder of Weighing; The rare earth oxide lysate is contained in the hold tank; With the rare earth oxide lysate, equivalent sprays equably in the pure molybdenum powder that is transported by auger by high-pressure spraying pump and spray header; After the preliminary mixing of auger,, send in the double spiral agitator by the compound import; Through after the mixing and stirring repeatedly of double spiral agitator, store by compound outlet fitted tube.
Described spiral spray design of Mixer parameter is: double spiral agitator diameter ∮ 800mm; Long 1200mm; Double spiral agitator shaft diameter ∮ 60mm; Double spiral agitator volume 0.59m
3Double spiral agitator axle rotating speed 12r/min; Motor power (output) 3KW; Mix churning time 30min; Loadings 85%.
Specific equipment hydraulic bidirectional harder in the described shaping treating processes comprises that press table oriented chute, mould top board, upper cylinder pressure head, upper cylinder, upper cylinder support, machine pillar, upper cylinder oil pipe, lathe are handled controlling box on bed piece, following oil cylinder oil pipe, following cylinder bracket, following oil cylinder, platen face, following oil cylinder pressure head, mould press table, plate shape blank shaping dies, the mould; The following oil cylinder oil pipe of oil cylinder under the described connection, cylinder bracket is arranged in the bed piece down, connect the following oil cylinder pressure head of oil cylinder down be arranged on the platen face above; Described mould press table, mould top board and plate shape blank shaping dies are connected, and plate shape blank shaping dies is provided with press table oriented chute on the mould; The upper cylinder pressure head of described connection upper cylinder, upper cylinder support, upper cylinder oil pipe are arranged on the machine pillar, and lathe is handled above-mentioned working part work of controlling box control.
Working process is: lathe is handled controlling box control hydraulic work system, realize upper cylinder pressure head and following oil cylinder pressure head from upper and lower both direction to be equal to pressure, slowly promote mould top board and mould press table simultaneously and do to move in opposite directions, progressively the molybdenum-based rare-earth alloy mixed powder that is seated in the plate shape blank shaping dies inner chamber is pressed into the molybdenum-based rare-earth alloy slab blank along the directed chute of clamping cap.
Add man-hour forming treatment process, at first according to consume factors such as the scaling loss in finished product parameters such as the density of molybdenum-based rare-earth alloy slab, thickness, planar dimension and sintering, the saw lumber course of processing, edgings, after calculating required molybdenum-based rare-earth alloy powder weight, weigh and get the raw materials ready; And then dimensional parameters and the shaping factors such as reservation porosity (general plate shape base material porosity select 40%), density required according to the shaping blank, adjust length and width, the thick dimensional parameters of setting plate shape blank mold; Adorn mould at last, pressed compact is shaped.
Because the molybdenum-based rare-earth alloy powder is in the pressurized forming process, along with the continuous increase of pressure, displacement and distortion by a relatively large margin can appear in powder particle; In displacement and deformation process, because mechanical interlocking and surface atom gravitation between the powder particle are all being had an effect, the connecting forces between the powder particle is progressively strengthened, blank has certain density and certain intensity gradually.But because pressurization is too fast, pressure is uneven or stressed deficiency, understands some particle recoverable deformation has only taken place, after external force is eliminated, powder particle will restore to the original state, and expanding or cracking will appear in blank; Therefore must make compacting pressure surpass the elastic limit of powder particle or keep the long duration under elevated pressures that (process parameters design is: pressure is greater than 30MPa, the voltage stabilizing time is more than 40min), impel powder particle generation viscous deformation or brittle rupture, just can guarantee the blank inner quality.In addition, behind the molybdenum-based rare-earth alloy slab blank press forming, need warehouse-in to deposit certain hour (process parameters design was: greater than 10 days) and make it weathering, also can slowly clear up or receive the internal stress that produces in the pressing process naturally, favourable raising molybdenum-based rare-earth alloy slab blank inner quality.
The present invention has the following advantages and positively effect:
1, the present invention adds a certain proportion of 4 kinds of rare earth oxides by blending simultaneously in pure molybdenum powder, utilize the rare earth alloy element to have the strong characteristic of the crystal grain of growing up, sink-resistance performance and creep property, pass through dispersion-strengthened action, improve the recrystallization temperature of metal molybdenum, improve the mechanical propertys such as tension, surrender, extension of molybdenum base material; Its manufacturing process is by complete science such as batching, mixing, shaping, sintering, saw lumber, advanced reasonably processing treatment process, spiral by special use sprays equipment such as mixing tank, hydraulic bidirectional harder, can satisfy the processing technology parameter of manufacturing process technology requirement, realization can produce the molybdenum-based rare-earth alloy slab with good mechanical properties, fill the domestic gaps, substitute imported materials and items.
2, in pure molybdenum powder, mix ZrO simultaneously
2Y
2O
3La
2O
3Nd
2O
3Deng 4 kinds of rare earth oxides, and research and design goes out the mixed ratio of science.This original creation mix kind and ratio, can fully effectively utilize rare earth element to have to grow up the strong characteristic of crystal grain, sink-resistance performance and creep property, by the rare earth element dispersion-strengthened action, improve the recrystallization temperature of molybdenum base material, thereby improve mechanical propertys such as molybdenum-based rare-earth alloy slab room temperature fragility and tension, extension, surrender, improve the environmental adaptation scope of molybdenum-based rare-earth alloy slab.
3, designed " spiral spray mixing tank " blending Technology specific equipment can solve the technical barrier of rare earth oxide blending skewness preferably, establishes the good technique basis for guaranteeing rare earth element uniform distribution, raising thing phase dispersing uniformity in molybdenum base material; Can guarantee simultaneously that the molybdenum-based rare-earth alloy powder that mixes the back gained presents: globule size is unified, constituent element is evenly distributed, do wet appropriateness, loose, and does not have the perfect condition of defectives such as caking or globe.
4, realize that by " hydraulic bidirectional harder " two pressure heads can be from upper and lower both direction to be equal to pressure, slowly the molybdenum-based rare-earth alloy powder in being seated in blank mold is exerted pressure simultaneously, is pressed into the molybdenum-based rare-earth alloy slab blank.The forming technology technology and the specific equipment of this original creation can be guaranteed molybdenum-based rare-earth alloy slab blank pressurized general equilibrium, and density distribution is even, and structural strength is bigger, can be the processing of operations such as following sintering, saw lumber, and high-quality basis blank is provided.
5, in the sintering processes process of molybdenum-based rare-earth alloy slab, according to the tabular characteristics of blank, creationary designing before carrying out blank sintering processing treatment, the newly-increased art treatment that at first in hydrogen atmosphere, toasts.The processing method of this innovation, residual aqueous vapor in the time of can removing molybdenum powder preferably and mix, the internal stress that produces in the time of also can effectively eliminating press forming can also be reduced certain rare earth oxide.By this innovative technology method, can effectively improve the quality product of molybdenum plate blank when sintering, rolling becoming a useful person.
6, in the saw lumber treating processes of molybdenum-based rare-earth alloy slab, according to the tabular characteristics of blank, the creationary innovation rolling methods such as horizontal breaking down, intersection warm-rolling of designing; Also creatively design the cogging breaking down, intersect various technology running technology parameters such as warm-rolling, three grades of rolling new technologies of segmentation such as accurate cold rolling and rolling fire, every fire time Heating temperature, heat-up time, fire time rolling pass, pass reduction, rolling direction, annealing temperature, annealing time; Also creationary designing in accurate cold rolling process simultaneously newly-increasedly added lubricant, rolled finishing process such as polishing surface plate; Creatively design stocking after annealed technology, all must pass through the newly-increased technological measure of alkali cleaning again.These that adopt in the saw lumber operation are innovated rolling means and technical data, can make the molybdenum-based rare-earth alloy slab goods increase density, strengthen plasticity, improve mechanical property, reduce surfaceness, improve surface smoothness and quality grade.
Metal molybdenum has fusing point height (2620 ℃), and electrical and thermal conductivity performance is good, and excellent specific properties such as hot strength and hardness are arranged; But also there is recrystallization temperature low (1100 ℃) in metal molybdenum, and weave construction and is raise and sharply grows up with temperature by the fibrous equi-axed crystal that is transformed into behind the recrystallize, easy brittle failure, easy major defect such as oxidation occur.In long term production, people find gradually, add after some element in metal molybdenum, can improve the recrystallization temperature of metal molybdenum, thereby improve some characteristic of metal molybdenum, improve mechanical property, enlarge use range, increase the service life.
The present invention through repeatedly research trial, contrast screening, determines to mix simultaneously ZrO according to the molecular structurology principle at last in pure molybdenum powder
2Y
2O
3La
2O
3Nd
2O
3Doped scheme Deng 4 kinds of rare earth oxides.Select to determine to mix simultaneously these 4 kinds of rare earth oxides and be because: they all have high melt point and boiling point (ZrO
22715/4840 ℃; Y
2O
32410/4300 ℃; La
2O
32300/4200 ℃; Nd
2O
32272/4050 ℃), can at high temperature keep basic synchronization deformation with molybdenum base parent metal material, but can not be dissolved in the fertile material; And the crystal grain during their recrystallize arranges vertically, is the long brilliant trivial bridging arrangement that connects of dovetail shaped behind the recrystallize, has sink-resistance performance and creep property preferably, and the metal molybdenum grain growth is had stronger restraining effect and dispersion-strengthened action; And these rare earth elements also have different characteristics such as different deep drawing qualities, plasticity, oxidation-resistance separately.Therefore, the above-mentioned 4 kinds of rare earth oxides that mix can increase substantially the recrystallization temperature (evidence can reach 1800 ℃) of molybdenum-based rare-earth alloy slab, improve room temperature and use mechanical property, improve high-temperature oxidation resistance, enlarge use range.
Description of drawings
Fig. 1 is a molybdenum-based rare-earth alloy slab manufacturing process flow diagram of the present invention
Fig. 2 is spiral spray mixer structure principle schematic of the present invention
Fig. 3 is two-way harder structural principle synoptic diagram for the present invention presses
Embodiment
Manufacture M
0100 of XB--2 * 450 * 800 (mm) molybdenum-based rare-earth alloy plates.
One, as shown in Figure 1: the first step processing of preparing burden: this treating processes is to carry out the based process process that group element material is prepared for manufacturing molybdenum-based rare-earth alloy slab.
Batching doped scheme of the present invention is: mix ZrO in pure molybdenum powder
2Y
2O
3La
2O
3Nd
2O
3Deng 4 kinds of rare earth oxides.
Optimum proportion doping ratio of the present invention is: 100 parts of pure molybdenum powders, ZrO
20.5 part, Y
2O
32 parts, La
2O
3: 2.5 parts, Nd
2O
3: 1 part.
According to manufacturing M
0XB--2 * 450 * 800 (mm) molybdenum-based rare-earth alloy board finished product volume and finished product density 10.15g/cm
3Criterion calculation, finished product net weight 7.3kg.
According to the batching that occurs in the manufacturing process, mixing, shaping consumption, warm-rolling is cut the limit and is cut damage, and finish rolling is cut the limit shaping and cut consumes such as damage, comprehensive coefficient of losses 10.1%; Molybdenum-based rare-earth alloy plate monolithic raw material is 8.12kg by norm, manufactures 100 tablet raw material norm quota of consumption total amount 812kg.
Allocate into according to the optimum proportion ratio of mixing up: the pure molybdenum powder that pure molybdenum powder 766.04kg selects to allocate into must meet standard GB/T3461-2006 requirement, and metal molybdenum content is greater than 99.9%, mean particle size range 6～10 μ m; ZrO
23.83kg, Y
2O
315.32kg, La
2O
319.15kg, Nd
2O
37.66kg。4 kinds of rare earth oxides that selection is allocated into all must meet the first grade quality standard requirement of manufacturing enterprise.
By the ZrO that allocates into
2, Y
2O
3, La
2O
3, Nd
2O
32.8 times of 4 kinds of rare earth oxide gross weight 45.96kg, allocate 128.69kg distilled water into, add the processing of sizing mixing in general " the heated and stirred dissolving vessel " that disposes, use the rotating speed of 86r/min when sizing mixing, temperature with 40～50 ℃, with the time of 50～60min, fully dissolve whole rare earth oxides.Then with the rare earth oxide lysate, the filtering net that reinjects selects to meet the mesh screen in safe diligent standard 120 mesh sieve holes.Removed the rare earth oxide behind impurity and the indissoluble thing, standby in the rare earth oxide lysate hold-up vessel 5 of pack into " spiral spray mixing tank ".
Two, as shown in Figures 1 and 2, second step was carried out combination treatment.Combination treatment is for manufacturing the molybdenum-based rare-earth alloy plate, preparing the processes technical process of molybdenum-based rare-earth alloy powder.
The combination treatment processes technology of the present invention's design, be in molybdenum powder, evenly to spray above-mentioned 4 kinds of rare earth oxide lysates, adopt a solid liquid Mixing Technology method, original creation design " spiral spray mixing tank " specific equipment by configuration and general " horizontal vibrations oven dry sieve " are realized.
" spiral spray mixing tank " specific equipment of original creation design, be by auger motor (1), auger (2), pure molybdenum powder charging opening (3), spray header (4), rare earth oxide lysate hold-up vessel (5), high-pressure spraying pump (6), double spiral agitator motor (7), compound import (8), double spiral agitator (9), compound outlet (10), form etc. main working parts, main technical details is: auger (2) diameter 400mm, long 1200mm, central siphon diameter of phi 80mm, rotating speed 18r/min, double spiral agitator (9) diameter 600mm, long 1200mm, central siphon diameter of phi 120mm, rotating speed 24r/min, power of motor 1.5kw, filling rate≤85%.The main technical details of general " horizontal vibrations oven dry sieve " is: oven dry: an electric heating element heating, spiral drying cylinder diameter of phi 600mm, long 1800mm, auger rotating speed 10r/min, 70～80 ℃ of bake out temperatures, drying time 80～90min; Pulverize: blade screw is pulverized, and blade rotational speed 40r/min, screen overflow can repeat to pulverize; Screening: the reciprocal reciprocating sieve of multilayer, the 120 times/min frequently that shakes, amplitude 10～35min, safe diligent standard 80 mesh sieve holes, sieving capacity 20kg/h.
Principle of work is: pure molybdenum powder is evenly delivered on the auger (2) by charging opening (3), start motor (1) and make auger (2) uniform rotation, promoting pure molybdenum powder at the uniform velocity advances, simultaneously, start high-pressure spraying pump (6), make the rare earth oxide lysate that is stored in the rare earth oxide lysate hold-up vessel (5) by spray header (4), evenly spray is on the pure molybdenum powder that is transported by auger (2).Transport in the process at auger (2), pure molybdenum powder and rare earth oxide lysate are rotating and are pushing under two kinds of actings in conjunction of cooperating to exert oneself, all taking place to overturn voluntarily and rolling complicated running orbit such as advance separately, therefore tentatively mixed, and, be sent in the double spiral agitator (9) by compound import (8); Because the specific function of double spiral agitator (9) can make to have obtained pure molybdenum powder of preliminary blended and rare earth oxide lysate, can obtain stirring two-way the mixing repeatedly.Pure molybdenum powder and rare earth oxide lysate, in double spiral agitator (9), with the speed of rotation of 24r/min, with 50～60min time, after the two-way stirring of mixing repeatedly, quilt is blended together is molybdenum-base rare earth oxide compound mixed ingredients.And discharge fitted tube by mixed ingredients outlet (10) and keep in, must not surpass 24h between fitted tube is temporary.
Then, molybdenum-base rare earth oxide compound mixed ingredients is sent in general " the horizontal vibration drying sieve " of configuration, after drying, pulverizing, sieve processing, obtain the molybdenum-based rare-earth alloy powder that blending powder appropriateness, constituent element were evenly distributed, did wet appropriateness, loose nothing caking.The molybdenum-based rare-earth alloy powder is answered the fitted tube sealing, and the warehouse-in keeping is stand-by.
Three, shown in accompanying drawing 1 and accompanying drawing 3, the 3rd goes on foot the processing that is shaped.The processing that is shaped is to be to manufacture the molybdenum-based rare-earth alloy plate, the processes technical process of preparation powder plate shape blank.
The shaping treatment process processing technology of the present invention's design, be to adopt the closely knit forming technique method of bidirectional hydraulic, the molybdenum-based rare-earth alloy powder pushed the plate shape blank that closely knit one-tenth has definite shape, size, porosity and intensity by the original creation design " hydraulic bidirectional harder " of configuration.Creating " hydraulic bidirectional harder " specific equipment of design, is to handle controlling box (27) by bed piece (11), following oil cylinder oil pipe (12), following cylinder bracket (13), following oil cylinder (14), platen face (15), following oil cylinder pressure head (16), mould press table (17), blank shaping dies (19), clamping cap oriented chute (20), mould top board (21), upper cylinder pressure head (22), upper cylinder (23), upper cylinder support (24), machine pillar (25), upper cylinder oil pipe (26), lathe; (described lathe is handled controlling box (27) and comprised toothed gear pump, draws and joins valve, surplus valve, safety valve, rate of flow meter, tensimeter, hydraulic efficiency oil fuel tank, motor etc.) working part is formed.Main technical details is: work top 600 * 1800mm, oil cylinder operating pressure 5000KN, liquid maximum working pressure (MWP) 32mpa, oil cylinder piston range 280mm, oil cylinder piston working speed 8mm/min, liquid peak flow 100L/min, power of motor 10kw.
At first, the molybdenum-based rare-earth alloy powder that is shaped required is got the raw materials ready.According to aforementioned calculation result, produce 100 molybdenum-based rare-earth alloy plate net weight 730kg, all comprehensive coefficient of losses 10.1%, wherein batching is handled coefficient of losses 0.3%, is shaped to handle and still have 9.8% with the comprehensive coefficient of losses of post-treatment.Calculate in view of the above, need molybdenum-based rare-earth alloy powder 809.3kg.
Secondly, according to monolithic molybdenum-based rare-earth alloy board finished product volume 720cm
3Radix, consider accurate cold rolling back cut edge loss, the vertical factors such as loss, each passage processing closely knit contraction in back and sintering shrinkage of cutting edge behind the warm-rolling one by one, calculate plate shape blank shaping volume and length each to size.As calculated: plate shape blank (high * wide * long) 65 * 310 * 430mm; Volume 8664cm
3Data are adjusted height, wide, long parameter that plate forms the shape dies cavity in view of the above, after setting mold work position stop means, begin to load the molybdenum-based rare-earth alloy powder.
Then, on " the hydraulic bidirectional harder " of configuration, push closely knit forming operation.Rely on the advanced function of hydraulic efficiency system, make upper cylinder pressure head (23) and the following oil cylinder pressure head (16) can both be with the working speed of 8mm/min with greater than the operating pressure of 30Mpa, from upper and lower both direction, with with equipressure and speed, slowly promote mould top board (21) and mould press table (17) simultaneously, do move toward one another along clamping cap oriented chute (20), gradually the molybdenum-based rare-earth alloy powder that is seated in blank shaping dies (19) inner chamber is pushed closely knit one-tenth 65 * 310 * 430mm plate shape blank.Simultaneously, when the upper and lower pressing plate (21,17) of blank shaping dies (19) is advanced to mold work position stop means, stop naturally moving; At this moment, upper and lower oil cylinder (23,14) still with the operating pressure greater than 30Mpa, keeps more than the voltage stabilizing 40min, to guarantee the density and the intensity of plate shape blank on this position.
At last, plate shape blank also must be put in storage and be deposited more than 10 days, carries out other manufacturing procedures after making it weathering again and handles.
Four, as shown in Figure 1, the 4th step was carried out sintering processes.Sintering processes is for manufacturing the molybdenum-based rare-earth alloy plate, the processes technical process of preparation processing saw lumber base material
At first, general " the hydrogen atmosphere roaster " by configuration is placed on plate shape blank body and carries out low-temperature bake in the hydrogen atmosphere and handle.700 ℃ of baking top temperatures; 8 ℃/min of temperature rise rate; Go into stove baking full time 240min; Cut off the power supply cooling cooling naturally in stove after reaching storing time; The storing time hydrogen flowing quantity is 〉=0.8m
3/ h.
Then, general " the hydrogen atmosphere sintering oven " by cultivating.Again plate shape blank body is placed in the hydrogen gas oxygen, carries out sintering processes with sufficient temp.1050 ℃ of presintering top temperatures; 20 ℃/min of temperature rise rate; Go into stove presintering full time 260min; Cut off the power supply cooling cooling naturally in stove after reaching the presintering time; Hydrogen flowing quantity 〉=1.5m during presintering
3/ h.
At last, general " the pre-induction sintering oven during hydrogen atmosphere is horizontal " by configuration is placed on plate shape blank body in the hydrogen atmosphere, carries out the finalization sintering processes with comparatively high temps.1850 ℃ of intermediate frequency sintering top temperatures; Temperature rise rate takes the segmentation variation pattern to heat up: 15 ℃/min * 50min; 10 ℃/min * 40min; 18 ℃/min * 40min, go into stove sintering full time 360min; Cut off the power supply cooling cooling naturally in stove after reaching sintering time; Hydrogen flowing quantity 〉=2m during sintering
3/ h.
Through behind the final sintering setting treatment, the powder plate shape blank of 65 * 310 * 430mm is shunk fine and close shrinking percentage reach 22.93%.Through the processing saw lumber blank of final sintering setting treatment, also must put in storage and deposit more than 15 days, carry out other saw lumber processing treatment again after making it weathering.
Five, as shown in Figure 1: the 5th step was carried out saw lumber processing.Saw lumber processing is the processes technical process that processing saw lumber blank is changed into molybdenum-based rare-earth alloy plate commodity.
At first, processing saw lumber blank is carried out cogging and go out to roll processing.
53 * 300 * 420mm processing saw lumber blank, general " in the hydrogen atmosphere process furnace " of putting configuration into carries out the heating first time.Heating and temperature control is controlled at 80～90min heat-up time, hydrogen flowing quantity 〉=0.8m at 1200～1300 ℃
3/ h after for the first time heating is finished, puts the base material on general " the four roller reversible hot rollss " of configuration into immediately and opens the wind breaking down.Hot mill rolling power 〉=450 ton, roll Φ 380 * 800mm, rolling working speed≤60m/min first fire all by base material horizontal direction carry out continuously toward anti-3 passages rolling after, form the not exclusively sheet material of 22 * 350 * 526mm of rule, total working modulus 39.35%, average pass reduction 13.11%.
After rolling the finishing, 22 * 350 * 526mm sheet material is put into again carried out the heating second time in " process furnace " immediately for the first time.Heating and temperature control is controlled at 40～50min heat-up time, hydrogen flowing quantity 〉=0.8m at 1100～1200 ℃ for the second time
3/ h after heating is finished for the second time, carries out the cogging breaking down second time to sheet material immediately in putting " hot rolls " into.Second fiery rolling working speed≤60m/min, still all come and go by the sheet material horizontal direction 3 passages rolling after, form the not exclusively sheet material of 10 * 386 * 539mm of rule, total working modulus 48.63%, average pass reduction 16.21%.
After rolling the finishing of second fire, 10 * 386 * 539mm sheet material is put in general " the hydrogen atmosphere annealing furnace " of configuration carried out anneal immediately.850 ± 10 ℃ of annealing temperatures, annealing soaking time 40min ± 5min, hydrogen flowing quantity 〉=0.5m
3/ h reaches annealing and cuts off the power supply after the soaking time, and sheet material naturally cooling " annealing furnace " in is lowered the temperature.
Put into after the sheet material cooling in " alkaline bath " of configuration and carry out clean.Alkaline wash is allocated with 30% KOH and tap water, and the alkaline wash temperature is controlled at 60～70 ℃.
Then, the sheet material through the cogging breaking down being carried out vertical warm-rolling handles.
The first rolling sheets of the cogging of 10 * 386 * 539mm, put and carry out first time in general " process furnace " of configuration and heat.Heating and temperature control is controlled at 70～80min heat-up time at 950～1050 ℃, hydrogen flowing quantity 〉=0.8
3/ h.After for the first time heating is finished, sheet material is put on " hot rolls " of configuration carried out vertically warm-rolling of first fire immediately.Rolling working speed≤60m/min, all come and go continuously by the sheet material longitudinal direction 3 passages rolling after, form the not exclusively sheet material of 5.6 * 408 * 619mm of rule, total working modulus 32.02%, average pass reduction 10.67%.
After rolling the finishing of first fire, 5.6 * 408 * 619mm sheet material is put into again carried out the heating second time in " process furnace " immediately.Heating and temperature control is controlled at 40～50min heat-up time, hydrogen flowing quantity 〉=0.8m at 900～1000 ℃ for the second time
3/ h.After heating is finished for the second time, sheet material is put in " hot rolls " immediately again, carried out vertically warm-rolling of second fire.The second fiery roll speed is still selected 60m/min, still all undertaken continuously coming and going by the sheet material longitudinal direction 3 passages rolling after, form the not exclusively sheet material of 3.6 * 438 * 697mm of rule, total working modulus 22.39%, average pass reduction 7.46%
After rolling the finishing of second fire,, put in " annealing furnace " of configuration and carry out anneal immediately 3.6 * 438 * 697mm sheet material.850 ± 10 ℃ of annealing temperatures, annealing soaking time 40min ± 5min, hydrogen flowing quantity 〉=0.5m
3/ h reaches annealing and cuts off the power supply after the soaking time, and sheet material is lowered the temperature naturally " annealing furnace " in and cooled off.
Put into after the sheet material cooling in " alkaline bath " of configuration and carry out clear processing, alkaline wash is allocated with 30% KOH and tap water, and the alkaline wash temperature is controlled at 60～70 ℃.
Warm-rolling sheet material is delivered on general " plate shearer " of configuration after alkaline wash cleans, and carries out preliminary correction of the flank shape and cuts the limit, excises the surplus limit that irregular calendering is protruded.Be cut into the back and form 3.6 * 422 * 680mm sheet material, cut the limit and cut loss rate 6.01%.
At last, the sheet material through vertical warm-rolling is carried out accurate cold-rolling treatment.
Earlier, smear cold-rolling lubricant, put then that to carry out first time precision in general " the four rod reversible precise cold milling trains " of configuration cold rolling into cotton yarn through cutting the warm-rolling plate surface of limit correction of the flank shape.400 tons of the precise cold mill rolling forces of configuration, roll 230 * 550mm, roll speed 60m/min.For the first time accurate cold rolling all by the sheet material longitudinal direction carry out coming and going continuously 4 passages rolling after, form the not exclusively sheet material of 2.6 * 442 * 724mm of rule, total working modulus 19.46%, average pass reduction 4.86%.
Finish for the first time accurate cold rolling after, on general " surface polishing machine " of configuration, after precise cold rolling sheets surface carried out polished finish, smear one deck cold-rolling lubricant again, put still then that to carry out the second time on " the precise cold milling train " of configuration accurate cold rolling into.Accurate cold rolling for the second time, it is rolling still all to be undertaken coming and going 3 passages continuously by the sheet material longitudinal direction, forms the not exclusively sheet material of 2 * 468 * 836mm of rule, total working modulus 5.96%, the average working modulus 1.98% of passage
Finish for the second time accurate cold rolling after, deliver on general " sheet shears " of configuration, by enterprise the dispatch from the factory specification and the deviation requirement of standard, cut the sheet material that the limit is configured as 2 * 450 * 800mm, cut the limit and cut loss rate 8%, as all execution is upward poor in accordance with regulations, then be configured as the sheet material of 2 * 460 * 815mm, cut the limit and cut loss rate 4%.
Cut the limit also after the shaping finishing, also will carry out the end product processing of sheet material according to producing requirement, comprising: work such as stickup are smeared, indicated to surface finish, antioxidant.
After finishing above-mentioned whole work, after quality testing department was inspected for acceptance, the packing warehouse-in was treated pin.
Claims (5)
1. the manufacturing process of a molybdenum-based rare-earth alloy slab, it is characterized in that: this molybdenum-based rare-earth alloy slab is handled five manufacturing technology steps by batching processing, combination treatment, shaping processing, sintering processes, saw lumber and is finished realization, and described molybdenum-based rare-earth alloy slab is by mix ZrO simultaneously in pure molybdenum powder
2, Y
2O
3, La
2O
3, Nd
2O
3Four kinds of oxide compound manufacturings form, and its each proportion of raw materials is: 100 parts of pure molybdenum powders, ZrO
20.5 part, Y
2O
32 parts, La
2O
3: 2.5 parts, Nd
2O
3: 1 part;
Concrete manufacturing process is as follows:
1., batching is handled: this treating processes is to carry out the based process process that group element material is prepared for manufacturing molybdenum-based rare-earth alloy slab, proportionally chooses raw material, pure molybdenum powder, ZrO
2, Y
2O
3, La
2O
3, Nd
2O
3, adopt the distilled water method of sizing mixing, add up to 2.8 times of gross weights to be equipped with distilled water according to whole oxide compounds of Weighing, the whole oxide compounds of dissolving in the heated and stirred dissolving vessel, and then filter by hay tank, remove impurity, make the lysate that contains four kinds of oxide compounds;
2., combination treatment: this treating processes is to handle for molybdenum-based rare-earth alloy slab is shaped, and prepares a kind of processes manufacturing processed of molybdenum-based rare-earth alloy powder; Described combination treatment process is to mix four kinds of oxide dissolution liquid by the even spray of spiral spray mixing tank in pure molybdenum powder, and then with the material after the blending through horizontal vibration drying sieve dry, pulverizing, Screening Treatment, the molybdenum-based rare-earth alloy powder of making after combination treatment processing is contained in temporary for some time in the stainless steel cylinder; But the temporary time should be above 24 hours;
3., shaping is handled: this treating processes is the molybdenum-based rare-earth alloy powder that will be mixed and made into, and a kind of technology that closely knit one-tenth has the blank of definite shape, size, porosity, intensity adds treating processes; Main process is at first according to density, thickness, planar dimension finished product parameter and the sintering of molybdenum-based rare-earth alloy slab, the scaling loss in the saw lumber course of processing, edging consume factor, calculate required molybdenum-based rare-earth alloy powder weight after, weigh and get the raw materials ready; And then dimensional parameters and the reservation porosity required according to the shaping blank, plate shape base material porosity uses the shaping factor of 40% density, adjusts length and width, the thick dimensional parameters of setting plate shape blank mold; Adorn mould at last, the molybdenum-based rare-earth alloy powder compression that will be mixed and made into by the hydraulic bidirectional harder become pressurized general equilibrium, density distribution evenly, molybdenum-based rare-earth alloy slab blank that structural strength is bigger;
；
4., sintering processes: this treating processes is after the molybdenum-based rare-earth alloy slab blank body is heated in suitable atmosphere and temperature, shrink a kind of technological process of densification, intensity increase, physical and chemical performance raising steady change, main process is the molybdenum-based rare-earth alloy slab blank body of press forming, sinters no dirtyization of sizing in surface, the no hierarchical crack in inside into, the molybdenum-based rare-earth alloy slab goods base material of suitable density, intensity and physics of metals characteristic is arranged;
5., saw lumber is handled: this treating processes is molybdenum-based rare-earth alloy slab goods base material, finish a kind of processes manufacturing processed that turns to geometrical shape, weave construction, mechanical property, the processing performance of goods attitude to change from sintered state, main process is the molybdenum-based rare-earth alloy slab goods base material of finishing sintering processes, and processing and manufacturing becomes can be directly used in a kind of molybdenum-based rare-earth alloy slab kind of electronics, electric power, space flight, automobile, metallurgical production industry.
2. the manufacturing process of a kind of molybdenum-based rare-earth alloy slab according to claim 1, it is characterized in that: described sintering processes processes process is to adopt the sintering process method of baking, presintering, 3 different stepss of intermediate frequency sintering, realizes by " hydrogen atmosphere roaster ", " the hydrogen atmosphere pre-burning freezing of a furnace " and " the horizontal intermediate frequency sintering oven of hydrogen atmosphere " of configuration:
1., initial stage of sintering processes process, adopt the hydrogen atmosphere roaster in hydrogen atmosphere, to toast, the bond strength between metallic particles is increased, interatomic gravitation increases on the link surface, bonds the baking process parameter between particle:
Baking top temperature: 700 ℃
Temperature rise rate: 10 ℃/min
Storing time: 240min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 0.8m
3/ h;
2., mid-term of sintering processes process, adopt hydrogen atmosphere pre-burning freezing of a furnace in hydrogen atmosphere, to carry out presintering, form big intensity of activation, allow the amplitude of atomic vibration strengthen, make abundant atom enter atom reactive force scope; Impel atom to pass through evaporation, diffusion, flow, condense migration form, form crystal grain boundary at granular boundary, and crystal grain boundary is moved to granule interior, cause grain growth or move crystal grain is merged by crystal boundary, produce volume diffusion, surface diffusion and crystal boundary diffusion, the pre-sintering process parameter:
Presintering top temperature: 1050 ℃
Temperature rise rate: 20 ℃/min
Sintering time: 260min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 1.5m
3/ h;
3., the later stage of sintering processes process, in hydrogen atmosphere, use the horizontal intermediate frequency sintering oven of hydrogen atmosphere to carry out last sintering, make the atomic diffusion of blank body and move to flow and obtain more abundant carrying out, hole quantity and size are fully reduced, established good physical, chemistry, mechanical property obtain fully stable, the intermediate frequency sintering process parameter:
Intermediate frequency sintering top temperature: 1850 ℃
Temperature rise rate: 15 ℃/min * 50min
10℃/min×40min
15℃/min×45min
Sintering time: 360min
The type of cooling: outage nature cooling cooling in the stove
Hydrogen flowing quantity: 2m
3/ h.
3. the manufacturing process of a kind of molybdenum-based rare-earth alloy slab according to claim 1, it is characterized in that: described saw lumber treating processes takes cogging breaking down, intersection warm-rolling, accurate cold rolling three grades of segmentation rolling technology methods to realize concrete technical data:
Cogging breaking down: first fire: Heating temperature: 1150～1300 ℃
Heat-up time: 80～90min
Fire time rolling pass: 3 times
Pass reduction: 20%
Rolling direction: whole transverse rollings
Second fire: Heating temperature: 1100～1200 ℃
Heat-up time: 40～50min
Fire time rolling pass: 3 times
Pass reduction :≤15%
Rolling direction: whole transverse rollings
Anneal: annealing temperature: 900 ℃ ± 10 ℃
Annealing soaking time: 〉=40min
Intersection warm-rolling: first fire: Heating temperature: 950～1050 ℃
Heat-up time: 70～80min
Fire time rolling pass: 3 times
Pass reduction :≤12%
Rolling direction: vertically, laterally, vertically tandem rolling again
Second fire: Heating temperature: 850～950 ℃
Heat-up time: 40～50min
Fire time rolling pass: 3 times
Pass reduction :≤10%
Rolling direction: vertically, laterally, vertically tandem rolling again
Anneal: annealing temperature: 900 ℃ ± 10 ℃
Annealing soaking time: 〉=60min
Accurate cold rolling: finish rolling for the first time: last pass: 3 times
Pass reduction :≤5%
Rolling direction: all vertically rolling
Finish rolling for the second time: last pass: 2 times
Pass reduction :≤2%
Rolling direction: all vertically rolling.
4. the manufacturing process of a kind of molybdenum-based rare-earth alloy slab according to claim 2, it is characterized in that: described saw lumber treatment process process is after annealed operation, need pass through alkali cleaning again, alkaline wash is selected the KOH of proportioning 30% for use, and the alkaline wash temperature is controlled at 80 ℃～90 ℃.
5. the manufacturing process of a kind of molybdenum-based rare-earth alloy slab according to claim 1, it is characterized in that: described saw lumber treatment process process also needs by adding cold-rolling lubricant and polished finish being carried out on the cold rolled sheet surface, this finishing rolling technology method can effectively improve the surface quality rank of molybdenum-based rare-earth alloy slab, enlarges use range.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100562583A CN101423911B (en) | 2007-10-29 | 2007-10-29 | Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100562583A CN101423911B (en) | 2007-10-29 | 2007-10-29 | Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101423911A CN101423911A (en) | 2009-05-06 |
| CN101423911B true CN101423911B (en) | 2011-09-07 |
Family
ID=40614791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007100562583A Active CN101423911B (en) | 2007-10-29 | 2007-10-29 | Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101423911B (en) |
Families Citing this family (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728838B (en) * | 2011-04-13 | 2015-02-11 | 四平市北威金属技术研发有限公司 | Preparing method of molybdenum-based rare earth oxide powder metallurgical alloy wafer |
| CN102218535B (en) * | 2011-07-14 | 2014-05-14 | 金堆城钼业股份有限公司 | Sintering method for molybdenum product |
| CN102615282A (en) * | 2012-03-27 | 2012-08-01 | 苏州先端稀有金属有限公司 | Processing method for manufacturing wide molybdenum sheet |
| CN102626845B (en) * | 2012-03-27 | 2015-06-03 | 苏州先端稀有金属有限公司 | Molybdenum lanthanum alloy tray processing method |
| CN103898385A (en) * | 2012-12-27 | 2014-07-02 | 四平市天阔换热设备有限公司 | Large-sized powder-metallurgic molybdenum-based rare earth alloy plate blank and preparation technology thereof |
| CN105014062A (en) * | 2014-05-03 | 2015-11-04 | 四平市北威金属技术研发有限公司 | Powder warm-compaction near-net molded molybdenum-based rare earth alloy top and manufacturing technology thereof |
| CN104328301B (en) * | 2014-07-18 | 2016-08-31 | 河南科技大学 | A kind of preparation method of particle-reinforced molybdenum-base composite material |
| CN104624642B (en) * | 2015-01-12 | 2016-12-07 | 郑州通达重型机械制造有限公司 | A kind of sputtering target material milling method of big substance wide cut molybdenum plate band |
| CN105618768B (en) * | 2015-12-28 | 2018-09-25 | 安泰天龙（天津）钨钼科技有限公司 | A kind of preparation method of high-compactness pure tungsten, pure molybdenum and its alloy material |
| CN105903976B (en) * | 2016-04-28 | 2018-05-18 | 金堆城钼业股份有限公司 | A kind of doping method of molybdenum alloy |
| CN106271452B (en) * | 2016-08-31 | 2019-07-16 | 佛山朕华照明材料有限公司 | A kind of production method of the white molybdenum filament of halogen lamp |
| CN107099716B (en) * | 2017-03-02 | 2019-01-08 | 中广核研究院有限公司 | Interface enhancing molybdenum alloy and preparation method thereof |
| JP6898792B2 (en) * | 2017-06-26 | 2021-07-07 | 日本特殊陶業株式会社 | Ceramic members and their manufacturing methods |
| CN109848424B (en) * | 2018-12-03 | 2021-08-10 | 有研工程技术研究院有限公司 | Molybdenum foil for grid control pulse traveling wave tube grid mesh and preparation method thereof |
| CN109940158B (en) * | 2019-04-03 | 2020-05-12 | 中南大学 | Rapid preparation process of fine-grain molybdenum plate |
| CN112011710A (en) * | 2019-05-31 | 2020-12-01 | 全亿大科技（佛山）有限公司 | Molybdenum alloy, preparation method of molybdenum alloy and sintering carrier |
| CN110724867B (en) * | 2019-11-29 | 2021-12-03 | 河南科技大学 | ZrO (ZrO)2-Y2O3Enhanced TZM alloy and preparation method thereof, and composite powder and preparation method thereof |
| CN111690888A (en) * | 2020-05-28 | 2020-09-22 | 河南新开源石化管道有限公司 | Titanium alloy raw material bulldozes crowded material device |
| CN112195385B (en) * | 2020-10-16 | 2021-07-13 | 内蒙金属材料研究所 | High-temperature-resistant high-toughness molybdenum-based composite material and preparation method thereof |
| CN112453401B (en) * | 2020-12-04 | 2021-12-28 | 西安交通大学 | Method for reducing anisotropy of rare earth molybdenum alloy material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448461A (en) * | 2002-12-06 | 2003-10-15 | 中国科学院上海硅酸盐研究所 | Toughness-improved molybdenum disilicide base composite exothermic -body and preparing method thereof |
| CN1676648A (en) * | 2005-05-15 | 2005-10-05 | 王治国 | Molybdenum-base alloy and its preparing method |
| CN1948533A (en) * | 2006-11-10 | 2007-04-18 | 西安华钼新材料股份有限公司 | High temperature resistant, anti electric arc corrosion composite rare earth molybdenum alloy and its preparation method |
-
2007
- 2007-10-29 CN CN2007100562583A patent/CN101423911B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448461A (en) * | 2002-12-06 | 2003-10-15 | 中国科学院上海硅酸盐研究所 | Toughness-improved molybdenum disilicide base composite exothermic -body and preparing method thereof |
| CN1676648A (en) * | 2005-05-15 | 2005-10-05 | 王治国 | Molybdenum-base alloy and its preparing method |
| CN1948533A (en) * | 2006-11-10 | 2007-04-18 | 西安华钼新材料股份有限公司 | High temperature resistant, anti electric arc corrosion composite rare earth molybdenum alloy and its preparation method |
Non-Patent Citations (6)
| Title |
|---|
| 张久兴等.掺杂符合稀土氧化物的钼的组织与性能.稀土20 5.1999,20(5),22-26. |
| 张久兴等.掺杂符合稀土氧化物的钼的组织与性能.稀土20 5.1999,20(5),22-26. * |
| 朱爱辉等.轧制方式对Mo－1钼板组织和性能的影响.硬质合金23 2.2006,23(2),97-99. |
| 朱爱辉等.轧制方式对Mo-1钼板组织和性能的影响.硬质合金23 2.2006,23(2),97-99. * |
| 王新钢等.稀土高温钼板室温塑性韧性研究.稀有金属27 1.2003,27(1),80-82. |
| 王新钢等.稀土高温钼板室温塑性韧性研究.稀有金属27 1.2003,27(1),80-82. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101423911A (en) | 2009-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101423911B (en) | Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof | |
| CN106048374B (en) | A kind of infusibility high-entropy alloy/carbonization titanium composite material and preparation method thereof | |
| CN109338199B (en) | Ceramic particle reinforced high-entropy alloy and preparation method thereof | |
| CN102312132B (en) | Method for preparing Ni-W alloy by vacuum sintering | |
| CN102728838B (en) | Preparing method of molybdenum-based rare earth oxide powder metallurgical alloy wafer | |
| CN102021460B (en) | Method for preparing W-10Ti alloy target material by using cool isostatic pressing and liquid-phase sintering | |
| CN108642457A (en) | A kind of production method of advanced lines molybdenum target material | |
| CN102531612A (en) | Silicon nitride material and preparation method of heat insulating disc cover prepared from same | |
| CN113427003B (en) | Large-size tungsten rod and preparation method thereof | |
| CN105478771B (en) | A kind of manufacture method of inexpensive molybdenum tube target | |
| CN101343751A (en) | Electrolytic aluminium anode carbon block and manufacture method thereof | |
| CN107287459A (en) | A kind of fine grain titanium aluminium powder forming method | |
| CN104232995A (en) | High-toughness ultrafine-grain composite titanium alloy and application and preparation method thereof | |
| CN110146357B (en) | Preparation method of vanadium slag/calcium oxide diffusion couple | |
| CN102251162A (en) | Preparation method of high performance nanometer lanthanide oxide doped molybdenum-silicon-boron alloy | |
| CN101696474A (en) | Powder metallurgy preparation method for rare-earth containing oxide reinforcing phase titanium alloy | |
| CN1081242C (en) | Process for preparing TiNi-base marmem directly from elements powder | |
| CN104475747A (en) | Method for sintering preparation of tantalum powder for high-purity tantalum ingots by carbon reduction process | |
| CN103710576B (en) | The high-strength nickel niobium alloy material that a kind of scandium, tantalum strengthen | |
| CN116356173A (en) | High-strength high-entropy alloy binding phase nanoscale hard alloy and preparation method thereof | |
| CN102248580A (en) | Molding method of fine grain graphite | |
| CN105773074A (en) | Manufacturing method of molybdenum alloy boat | |
| CN104294077A (en) | SiC/Cu composite material and preparation method thereof | |
| CN103695718B (en) | The high-strength nickel niobium alloy material that a kind of zirconium, chromium strengthen | |
| CN102275905B (en) | EXT454 ultrafine-grained structure graphite and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |