CN109468480A - The method that the vacuum canning rolling of impulse electric field auxiliary prepares metal-base composites - Google Patents
The method that the vacuum canning rolling of impulse electric field auxiliary prepares metal-base composites Download PDFInfo
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- CN109468480A CN109468480A CN201811412613.0A CN201811412613A CN109468480A CN 109468480 A CN109468480 A CN 109468480A CN 201811412613 A CN201811412613 A CN 201811412613A CN 109468480 A CN109468480 A CN 109468480A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
Abstract
The invention discloses a kind of methods of metal-base composites of the pack rolling preparation containing reinforced phase of pulse current auxiliary, it include: that will be first superimposed after composite powder base and heat treatment with surface treated metal skin plates, and carry out the weldering of vacuum side and take out inner air to the greatest extent, form vacuum canning test specimen structure；Jacket test specimen is put into milling train later, and according to pack rolling process, the brush of the pulse power and different location is connected, applies electric current in jacket surface, the synchronous green compact plasma agglomeration that carries out is rolled with jacket Electroplastic.Rationally control current parameters roll rate and reduction ratio, through multiroll rolling and reasonable sintering time, obtain larger size metal-based compound plate.Vacuum canning is rolled and is coupled with impulse electric field by the present invention; it can be in a short time; it is sintered and roll forming macroscopic view large scale, microcosmic crystal grain is tiny, the high-performance plate of metal-based compound containing reinforced phase of the distribution of reinforced phase even dispersion, have the characteristics that efficient low-consume, scale and intensive manufacture.
Description
Technical field
The invention belongs to the pack rolling technical field under the auxiliary of outfield, specially a kind of Metal Substrate of pulse current auxiliary
Composite material molding technology of pack rolling while sintering, especially a kind of being rolled by jacket based on pulse current auxiliary
Jacket rolls while system production ceramics, the aluminium of graphene or carbon fiber particles reinforced phase, magnesium, copper, iron, titanium composite material sintering
Make molding method.
Background technique
The support of high-end equipment and manufacturing fast-developing too busy to get away high performance material, especially to the lighting of material,
The high parameters such as strong abrasion, Gao Qiangren, corrosion-resistant, high temperature resistant, function/structure-integrated propose more stringent requirement.Metal
Based composites are the inhomogeneous composite materials of the enhancing phase composition such as metal and ceramics, fiber or carbon nanotube particulate, embody gold
There is superhigh intensity while belonging to characteristic, be the important structure of national economy every field and tool materials.However, reinforced phase with
Ingredient, structure and the performance difference of metallic matrix greatly, lead to lower finished product toughness plasticity, machining difficulty, especially synthesis work
Skill is complicated, not only needs the high―temperature nuclei under vacuum or protective atmosphere, and is difficult to that large-scale or complex-shaped component is made, thus
It is seriously kept in check in the application of related fields.The preparation method of existing metal-base composites mainly have high-temperature vacuum sintering,
The methods of discharge plasma sintering, SHS process and hip moulding.Relevant research and application achieve larger
Progress, still, these methods can not prepare large volume component, and generally existing equipment requirement is high, at high cost, low efficiency and
The problems such as being difficult to realize large-scale production.In view of this, it would be highly desirable to one kind is developed under the conditions of vacuum or protective atmosphere, low cost,
The new method of scale, the efficiently metal-base composites of production larger size, meets every profession and trade to metal-base composites
Wilderness demand.
Powder jacket rolling technique can guarantee to roll powder and form under vacuum and the conditions of high temperature such as close, thus effectively keep away
Exempt from powder body material loss, oxidation and crystal grain to grow up, it is easy to accomplish integration and near-net-shape.But it is applied to metal-based compound
The preparation of material is but rarely reported, main reason is that reinforced phase such as ceramic particle and metallic matrix materialization difference are big, wetting is tired
Difficulty needs high temperature sintering and continues to keep the temperature, even if but high temperature pack rolling, temperature and soaking time be difficult to reach sintering mark
It is quasi-.
Summary of the invention
In order to using efficiently, low cost, can scale rolling mill practice obtain crystal grain it is tiny and it is large-sized contain reinforced phase
Metal-base composites component, pulse current is applied on multi-roll mill it is an object of the present invention to provide a kind of, carry out metal
The new method of forming and sintering part while based composites are powder sintered.This method is suitable for different ceramics, graphene or carbon
Fiber reinforcement phase and aluminium, magnesium, copper, iron or titanium simple substance (alloy) powder combinations, such as B4C ceramic particle and pure aluminium powder.
The present invention is achieved by the following technical scheme:
A kind of method that the vacuum canning rolling of impulse electric field auxiliary prepares metal-base composites, includes the following steps:
(1), prepared by raw material
It is mixed through mechanical ball mill with ceramics, graphene or fibre reinforced phase and simple substance (alloy) powder of aluminium, magnesium, copper, iron or titanium
Expect, atomic fraction shared by reinforced phase is 3% ~ 30%.
(2), heat treatment and high-temperature degassing
The mixed powder of reinforced phase and metal simple-substance or alloy is placed in vacuum or inert gas and is heated to metal simple-substance or alloy
The 50% ~ 90% of fusing point, soaking time 60min, then cools down.
(3), plate surface is handled
Close according to parent metal simple substance (alloy) selection and its intensity and high-temp plastic, the low sheath material of thermal conductivity is chosen
Sheet metal of the thickness between 0.5 ~ 3mm, which cut, is used as jacket cladding plate, makes 600 ~ 1200mm of panel length, width is
100~300mm。
The aqueous corrosion of sulfuric acid, nitric acid, hydrochloric acid, hydrofluoric acid according to oxide layer composition selection different ratio etc. cleans gold
Belong to plate and powder green compact surface to be contacted, then carries out the polishing of mechanical and sand paper and completely remove surface oxide layer and exposed surface
Fresh metal guarantees that surface roughness is 40 ~ 110 μm, removal surface and oil contaminant is cleaned multiple times with alcohol and acetone soln, to be dried
Waterglass is smeared on surface to be contacted afterwards and glass lubricant is spare.
(4), powder green compact is prepared
By step (2) obtain mixed-powder be sent into roll carry out powder rolling, rolling environment temperature be 20 ~ 80 DEG C, powder without
It needs to heat, a length of 597 ~ 1197mm of green compact size, width is 97 ~ 297mm, with a thickness of 1 ~ 15mm.
(5), vacuum canning test specimen assembles
It is stacked according to upper cladding plate/powder green compact/lower cladding plate sequence, is surrounded by soldering and sealing plate, wherein soldering and sealing plate in two sides is provided with
Vacuum hole, preposition in vacuum heating indoor degasification in jacket welding, heating temperature is 300 DEG C, soaking time 60min, then side
Cooling side carries out the welding of vacuum edge, constitutes jacket test specimen, and will be evacuated to vacuum, vacuum degree inside jacket test specimen by vacuum hole
Are as follows: low vacuum is evacuated to: 5 × 10-1Pa, high vacuum are evacuated to: 1 × 10-2Pa carries out vacuum seal to vacuum hole after test specimen is cooling
Weldering.
(6), it rolls and is sintered
Jacket test specimen is put into the milling train for being connected to pulse current, milling train is at least made of 3 groups of rolls, and jacket piece lengths are bigger
In first and last roll axis distance, the brush that can be contacted with jacket surface of test piece, metal are equipped with positioned at the two sides of upper layer roll
The sintering of based composites is the resistance heat generated between powder particle using pulse current and plasma discharge heat, positive direct-current arteries and veins
It rushes current feedback circuit generation electric current and forms current loop through being placed in the brush of jacket surface of test piece by high-voltage output end, ground terminal,
The on-off of current feedback circuit port and brush depends on the rolling run of jacket, basic principle be jacket region as much as possible with
The pulse power forms closed circuit, so that sintering time be maximized.Feeding process is as follows: the roll number of milling train is n, each group electricity
Brush can be connect by contact conductor with the output and ground of impulse current generator, and with the upper surface of jacket test specimen or
Following table face contact, before being distributed in first group of roll, after most end group roll and between each group roll, respectively brush 1, electricity
Brush 2 ..., brush n, be sequentially distributed from first group of roll to most end group roll；Jacket test specimen front end enter at first milling train and with
Start rolling after first group of roll contact, after front end and brush 2 contact, by brush 1 and brush 2 be respectively connected to output end and
Ground terminal, powder green compact is sintered in the jacket between brush 1 and brush 2 at this time；As jacket is fed, whenever front end starts
Contact certain brush m(2≤m≤n) while, brush m ﹣ 1 is disconnected, and connect brush m and ground terminal, until brush 1 and brush n points
Not Jie Ru output and ground, there is maximum sintering region at this time；Continue to feed, brush 1 is left in jacket rear end, disconnects brush
1 and connect brush 2 and output end, powder green compact is sintered in the jacket between brush 2 and brush n at this time, with rear end with
Certain brush k(k≤n ﹣ 2) separation, brush k+1 is connected while disconnecting brush k to output end, which can guarantee jacket test specimen
Internal powder green compact as much as possible is in sintering state.To reduce current loss, each group roll is made of insulating material, such as
Sialon ceramic roll.
Electric current is input to the workshop section to be added of jacket test specimen, plasma discharge occurs between jacket internal particle, temperature rises rapidly
The concurrent bioelement diffusion of high yield raw burn knot neck and interfacial reaction, the rapid densified sintering product of green compact under the synergistic effect of roll-force, institute
It states in mode, the effect of the fast lifting of temperature, roll-force and current activation makes crystal grain refinement, reinforced phase Mass distribution, shows
Work improves material toughness plasticity；Multi-pass is carried out by control pulse current parameter, rolling reduction ratio and rolling rate when rolling
Rolling, first rolling pass reduction are not less than 13%, and total reduction is 50% ~ 75%；According to the difference of agglomerated material, selection is suitably rolled
Pulse current parameter processed: 200 ~ 1000A/mm of pulse current density2, 300 ~ 3000Hz of frequency, 30 ~ 100 μ s of pulse width；To protect
Enough sintering times are demonstrate,proved, by taking 1000mm jacket test specimen as an example, mill speed 200mm/min, mill speed guarantees in jacket
Powder green compact has everywhere >=discharge plasma sintering time of 5min.Jacket test specimen internal material high temperature, draught pressure and
The quick metallurgical bonding, it can be achieved that between powder particle is descended in current activation effect, forms dense sintering material.
(7), sheath material cools down at room temperature, is down to 100 DEG C hereinafter, breaking jacket test specimen to temperature, taking-up pellet obtains
To ceramics, graphene or Carbon Fibre Reinforced Metal Matrix Composites.
Based on the above method, the metal-base composites pack rolling device of the impulse electric field auxiliary of use, including it is used for
Pulse current power supply, conduction and the Electical connector for applying pulse current to experimental material, for applying multiple tracks to experimental material
The milling train of secondary rolling.Pulse current power supply uses impulse current generator, and using IGBT as digital power module, ultracrystallite soft magnetism is closed
Golden material is transformer core, is furnished with voltage, electric current automatic feedback, system fault diagnosis defencive function, and current peak density is
1000A/mm2, pulse frequency is 100 ~ 3000Hz.
The present invention has the advantage that and effect compared with traditional technology:
1, the present invention combines external impulse electric field and multi-roll mill, the system for the metal-base composites containing reinforced phase
It is standby.Because pulse current is by composite material green compact, resistance heat and plasma discharge heat are formed as interface atoms in granular boundary
The main energetic of diffusion and metallurgical reaction is not necessarily to external radiations heat energy, only is brought rapidly up to form sintering neck in granular boundary, then
Cause elements diffusion and interfacial reaction between particle, environment temperature is lower, reduces energy consumption while greatly improving sintering efficiency.
2, the electron wind that electric pulse causes, can driving element spread and reduces the Apparent activation energy of interfacial reaction, improve original
Son diffusion and interfacial reaction growth rate.As the temperature at powder particle interface increases rapidly, when reaching metal or alloy fusing point
Afterwards, material generates liquid phase in contact microcell fusing, and under the synergistic effect in the rolling field of force, powder green compact fast densification is complete
At sintering, and multi- pass rolling is uniformly distributed sintered body crystal grain refinement, reinforced phase disperse.The association of impulse electric field and the rolling field of force
Same-action, roll forming while making green compact complete sintering, more for excellent comprehensive performance.
3, pulse current not only acts as agglomeration, can also cause the electro plastic effect of metal plate and green compact, thus aobvious
Writing reduces distortional stress, reduces roll-force, avoids roll from damaging while reducing energy consumption.
4, different from sintering is diffused using traditional vacuum sintering furnace, in such a way that pulse current assists pack rolling
Sintering and molding green compact, not will receive the limitation of narrow mold in sintering furnace, jacket sample dimensions are flexible, and the method is suitable for
The production of large scale metal-base composites component especially large size plate, it can be achieved that component large-scale production, have aobvious
The prospects for commercial application of work.
5, the present invention integrates the discharge plasma sintering and pack rolling technique of the metal-base composites containing reinforced phase
It combines together, pack rolling acceleration of sintering, electro plastic effect is conducive to rolling stress reduction again, forms the rolling field of force-pulse
Electric field-temperature field multi- scenarios method synergistic effect realizes that high efficiency, low cost, intensive, prepare with scale large scale Metal Substrate is multiple
The purpose of condensation material component.
The present invention has rational design, by pulse current Fast Sintering technology in conjunction with powder jacket rolling mill practice, proposes one kind
By the sintering of reinforced phase metal-base composites and the integrated new method of roll forming.This method fully utilizes pulse current
In the resistance heat and plasma discharge heat of heterogeneous interface generation, active element diffusion, the effect and jacket for promoting interfacial reaction
The effect in terms of maintaining vacuum, keeping the high temperature such as close, refine crystal grain and form larger size component is rolled, by metal-based compound
Material is placed under the multi- scenarios method effect of temperature field, pressure field and impulse electric field, realizes the fast of large scale metal-based compound component
Speed, low cost sintering rolling integration system are standby.
Detailed description of the invention
Fig. 1 shows the device signals that the pack rolling based on pulse current auxiliary in the present invention prepares metal-base composites
Scheme, arrow indicates rolling direction of feed in figure.
Fig. 2 indicates the structural schematic diagram of metal-base composites powder green compact jacket test specimen in the present invention.
In figure: 1- roller mill rack, first group of roll of 2-, 3- most end group roll, 4- middle groups roll, 5- brush I, 6- electricity
Brush II, 7- brush III, 8- brush IV, 9- impulse current generator, 10- output end, 11- ground terminal, 12- upper cladding plate covers under 13-
Plate, 14- soldering and sealing plate, 15- powder green compact, 16- weld seam, 17- vacuum hole, 18- jacket test specimen, a- jacket test specimen front end, b- jacket
Test specimen rear end.
Specific embodiment
Specific embodiments of the present invention are described in detail below.
A kind of method that the powder pack rolling of impulse electric field auxiliary prepares metal-base composites, comprising: first will be compound
It is superimposed after powder base and heat treatment with surface treated metal skin plates, and carries out the weldering of vacuum side and take out inner air to the greatest extent, shape
At vacuum wrapping structure, prevent green sintering from aoxidizing；Jacket is put into milling train later, and according to pack rolling process, by pulse
The brush of power supply and different location is connected, and applies electric current in jacket surface, synchronous progress green compact plasma agglomeration and jacket are electroluminescent
Plasticity rolling.
The component used in the method for the present invention includes powder green compact jacket test specimen structure, for rolling the multiple roll of wrapping structure
Milling train, the electric field for applying pulse current to wrapping structure occurs and conduction device.
As shown in Fig. 2, upper cladding plate 12, lower cladding plate 13 and powder green compact of the jacket test specimen structure by covering package powder green compact
15 and soldering and sealing plate 14 form.Powder green compact 15 is metal-base composites, such as B4C particle enhanced aluminum-based composite material.On
Lower cladding plate 12,13 is elemental metals or alloy material, and selection is close with dense material distortional stress corresponding to metallic matrix
Thin plate, with a thickness of 0.5 ~ 3mm, such as 2A50 aluminium alloy plate.Soldering and sealing plate 14 is in powder green compact 15 and upper and lower cladding plate 12,13 contact positions
The position of face is provided with gas vent 17, and welds with upper and lower cladding plate 12,13 vacuum edge.Become to reduce powder green compact 15 in rolling
Frictional force, deformation drag during shape between jacket cladding plate, and prevent green compact to be sintered with jacket cladding plate and be adhered, in upper and lower cladding plate
12,13 and the inside of soldering and sealing plate 14 uniformly smear waterglass+glass lubricant.
As shown in Figure 1, multi-roll mill is used to roll jacket test specimen, to the roll-force that test specimen applies, not only to powder green compact
The compression for being conducive to sintering is generated, green compact are more shaped to specified thickness plate structure.Milling train includes 1, first group of rack and rolls
Roller 2, middle groups roll 4 and most end group roll 3, and jacket piece lengths are slightly larger than first and last roll axis distance, each group roll is equal
It is made of insulating material, such as Sialon ceramic roller.Rationally control current parameters, first rolling pass reduction is not less than 13% when rolling, always
Reduction ratio is 50% ~ 75%, and rolling rate is 150mm/min ~ 200mm/min, when sintering through multiroll rolling and 5min ~ 8min
Between, obtain larger size metal-based compound plate.
As shown in Figure 1, impulse electric field application system is by Pulsed Electric Fields Generator 9,10 and of positive direct-current high voltage pulse output end
The brush number that the composition of ground terminal 11, output and ground terminal are connected depends on the rolling process of jacket test specimen, and principle is to allow to the greatest extent
Jacket more than possible is in pulse current loop, increases sintering time.It is illustrated by taking three-high mill as an example, specifically feeds process
As follows, jacket test specimen front end b enters milling train at first and starts rolling after contacting with first group of roll 2, when the end b and brush II 6 connect
After touch, brush I 5 and brush II 6 are respectively connected to output end 10 and ground terminal 11, at this time the packet between brush I 5 and brush II 6
Set test specimen region can be sintered；As jacket test specimen is fed, in front end b contact brush m(2≤m≤4) while, it disconnects
Brush m ﹣ 1, and brush m and ground terminal 11 are connected, until brush IV 8 and ground terminal 11 are connected；Continue to feed, after jacket test specimen
End a leaves brush I 5, then disconnects brush I 5 and connect brush II 6 and output end 10, at this time between brush II 6 and brush IV 8
Powder green compact can be sintered in jacket test specimen, and with feeding, rear end a is contacted and disconnected one by one with brush, as rear end a and electricity
Brush k(1≤k≤2) separation, brush k+1 is connected while disconnecting brush k to output end 10, until rear end a is separated with brush II 6,
Region between remaining brush II 7 and brush IV 8 is sintered, which can guarantee that jacket test specimen region as much as possible is in
Sintering state.
Pulse current density of the present invention is 200 ~ 1000A/mm2, 300 ~ 3000Hz of frequency, 30 ~ 100 μ of pulse width
S selects suitable pulse current parameter, basic principle is: plate according to different powder green compact materials and different jacket sizes
Material sectional dimension is smaller, and pulse current frequency then needs bigger；The strength of materials is higher, corresponding pulse width and current density amplitude
It needs to improve；Rolling deformation rate is bigger, and pulse width and current density amplitude need to increase accordingly.
In the embodiment that other pulse current auxiliary pack rollings of the invention prepare metal-base composites, each group is rolled
Roller is made of insulating material, and can be yttrium stable zirconium oxide ceramics.
In the embodiment that other pulse current auxiliary pack rollings of the invention prepare metal-base composites, milling train rolls
Roller group number can be 1 ~ 5 group, and first and last roll axis distance is slightly less than jacket piece lengths.
In the embodiment that other pulse current auxiliary pack rollings of the invention prepare metal-base composites, cover up and down
The material of plate should be matched with the distortional stress of green compact metallic matrix, can be one in magnesium, aluminium, titanium, iron elemental metals or alloy
Kind.
In the embodiment that other pulse current auxiliary pack rollings of the invention prepare metal-base composites, powder is raw
Blank material material can be the magnesium of graphene, carbon fiber, ceramic particle or whisker reinforcement, aluminium, iron, titanium, one in Cu-base composites
Kind.
Using being particularly advantageous in that for the method for the present invention: the sintering of metal-base composites and rolling plastic deformation simultaneously into
Row, pulse current flow through powder green compact, cause generation resistance heat, plasma discharge heat between powder particle, and temperature increases rapidly shape
At neck is sintered between particle, elements diffusion and interfacial reaction occurs, then interface is quickly cooled down, and soaking time is short.In pulse current
Field causes under effect and the synergistic effect in the rolling field of force, can prepare crystal grain refinement, consistency height and reinforced phase within a short period of time
Equally distributed metal-base composites；It is different from conventional sintering furnace vacuum-sintering, by the mode that vacuum canning welds, was both protected
Vacuum-sintering environment has been demonstrate,proved, the limitation of narrow mold in vacuum drying oven is in turn avoided, can prepare and has formed large scale metal-based compound
Material plate.
The method that prepared by metal-base composites to pulse current auxiliary vacuum canning of the invention below by embodiment
It is described in further detail.
Embodiment 1
Based on discharge plasma sintering and vacuum canning rolling preparation B4The method of C particle enhanced aluminum-based composite material, including such as
Lower step:
1, jacket is prepared
A, 15vol% B will be contained4The aluminum-based powder of C ceramic particle (10 ~ 70 μm) is added in the heating furnace full of inert gas,
It is heated to vacuum ball milling 1h under 500 DEG C of dryings and high-temperature degassing 2h, 300rpm revolving speed, through powder rolling at 997 × 60 × 1.5mm
Powder green compact；
B, 2A50 aluminium alloy plate is cut into the plate of 1000 × 63 × 2mm, corrodes cleaning metal plate using 10% aqueous sulfuric acid
Then material and powder surface to be contacted carry out the polishing of mechanical and sand paper and completely remove surface oxide layer and the fresh gold of exposed surface
Belong to, and guarantee that surface roughness is 40 ~ 110 μm, removal surface and oil contaminant then is cleaned multiple times with alcohol and acetone soln, it is to be dried
Waterglass is smeared on surface to be contacted afterwards and glass lubricant is spare；
C, treated green compact and metal plate according to aluminium alloy/green compact/aluminium alloy sequence alignment are stacked into composition composite layer assembly,
In composite layer side and soldering and sealing plate by argon arc welding welding, two are opened in soldering and sealing plate face aluminium skin alloys/green compact contact surface position
A vacuum hole, then extracts interlayer air, makes to form vacuum environment inside jacket, and vacuum seal vacuum hole.
2, pulse current and multi-roll mill type selecting
The producible maximum current peak density of impulse generator is 1000A/mm2, pulse frequency is 100 ~ 3000Hz；This implementation
Example uses 3 roller mills, and roll is all made of Sialon ceramic roller, and first and last roll axis distance is slightly less than jacket length 1000mm.
3, pulse current assists pack rolling
Jacket composite layer is put into the milling train for being connected to pulse current, impulse generator 9 is accessed into 220V alternating current, running parameter is set
It is set to current density 700A/mm2, pulse frequency 900Hz, 80 μm of pulse width, unbalanced pulse power supply is by pulse current through brush
It is transferred to be sintered and rolling section, brush connection sequence is as previously described.Each roll reduction ratio is respectively 18%, 34% and 50%, stagnation pressure
Lower rate is 50%, mill speed 150mm/min, it is ensured that in jacket powder green compact have everywhere >=electric discharge of 6min etc. from
Sub- sintering time.
4, composite material post-processes
Jacket cools down at room temperature, is down to 100 DEG C hereinafter, breaking metal plate to temperature, taking-up pellet obtains fine and close B4C pottery
Porcelain particle enhanced aluminum-based composite material is sintered plate, local diffusion layer of the surface through further mechanical grinding removal and cladding plate.
Embodiment 2
Based on the method that discharge plasma sintering and vacuum canning rolling prepare carbon nano-tube fibre enhancing magnesium-based composite material, packet
Include following steps:
1, jacket is prepared
A, the Al powder containing 2wt% carbon nanotube is added in the heating furnace full of inert gas, is heated to 500 DEG C of dryings and height
Warm degasification 2h, vacuum ball milling 2h under 300rpm revolving speed, through powder rolling at the powder green compact of 997 × 60 × 1.5mm；
B, 2A50 aluminium alloy plate is cut into the plate of 1000 × 63 × 2mm, corrodes cleaning metal plate using 10% aqueous sulfuric acid
Then material and powder surface to be contacted carry out the polishing of mechanical and sand paper and completely remove surface oxide layer and the fresh gold of exposed surface
Belong to, and guarantee that surface roughness is 40 ~ 110 μm, removal surface and oil contaminant then is cleaned multiple times with alcohol and acetone soln, it is to be dried
Waterglass is smeared on surface to be contacted afterwards and glass lubricant is spare；
C, treated green compact and metal plate according to aluminium alloy/green compact/aluminium alloy sequence alignment are stacked into composition composite layer assembly,
In composite layer side and soldering and sealing plate by argon arc welding welding, two are opened in soldering and sealing plate face aluminium skin alloys/green compact contact surface position
A vacuum hole, then extracts interlayer air, makes to form vacuum environment inside jacket, and vacuum seal vacuum hole.
2, pulse current and multi-roll mill type selecting
The producible maximum current peak density of impulse generator is 1000A/mm2, pulse frequency is 100 ~ 3000Hz；This implementation
Example uses 3 roller mills, and each group roll is all made of yttrium stable zirconium oxide ceramic roller, and first and last roll axis distance is slightly less than jacket length
1000mm。
3, pulse current assists pack rolling
Jacket composite layer assembly is put into the milling train for being connected to pulse current, the pulse power is accessed into 220V alternating current, running parameter
It is set as current density 600A/mm2, pulse frequency 800Hz, 60 μm of pulse width, unbalanced pulse power supply is by pulse current through electricity
Brush is transferred to be sintered and rolling section, and brush connection sequence is as previously described.Each roll reduction ratio is respectively 18%, 34% and 50%, always
Reduction ratio is 50%, mill speed 160mm/min, it is ensured that powder green compact has the >=electric discharge etc. of 5min everywhere in jacket
Ion sintering time.
4, composite material post-processes
Jacket cools down at room temperature, is down to 100 DEG C hereinafter, breaking metal plate to temperature, taking-up pellet obtains fine and close carbon nanometer
Pipe reinforced aluminum matrix composites are sintered plate, diffusion part and oxygen of the surface through further mechanical grinding removal sintered body and cladding plate
Change part.
The pack rolling of impulse electric field auxiliary prepares the working principle of metal-base composites: in temperature field-current activation-
Under the compound action for rolling the field of force, the discharge plasma sintering and Electroplastic of the metal-base composites of reinforced phase are synchronously completed
Roll forming.Firstly, pulse current generates contact resistance heat and plasma discharge heat through granular boundary, to replace extraneous heat
Source makes temperature between the metal-base composites particle containing reinforced phase be quickly raised to sintering temperature；Secondly, pulse current can be significant
Elements diffusion activation energy is reduced, interfacial reaction rate is promoted；Finally, burning powder green compact rapidly in conjunction with the multi- pass rolling field of force
While knot is fine and close, avoids reinforced phase reunion and crystal grain is grown up.Vacuum furnace body, sintered body ruler are replaced using vacuum canning structure
It is very little no longer to be limited by mold volumes, it is obviously improved sinterable volume, and realize roll forming while sintering.
Vacuum canning is rolled and is coupled with impulse electric field by the present invention, can be sintered in a short time and roll forming macroscopic view is big
The high-performance plate of metal-based compound containing reinforced phase that size, microcosmic crystal grain are tiny, reinforced phase even dispersion is distributed has efficiently low
The characteristics of consumption, scale and intensive manufacture.
The present invention is elaborated in conjunction with the accompanying drawings and embodiments above, but above illustrate is merely to illustrate the present invention,
Rather than present invention is limited in any form.And described embodiment is only a part of the embodiment of the present invention, rather than all
Embodiment, based on the embodiments of the present invention, those of ordinary skill in the art institute without making creative work
Obtained all other embodiment belongs to the range that the present invention is protected.
Claims (6)
1. a kind of method that the vacuum canning rolling of impulse electric field auxiliary prepares metal-base composites, it is characterised in that: including
Following steps:
(1), prepared by raw material
It is mixed through mechanical ball mill with ceramics, graphene or fibre reinforced phase and simple substance (alloy) powder of aluminium, magnesium, copper, iron or titanium
Expect, atomic fraction shared by reinforced phase is 3% ~ 30%；
(2), heat treatment and high-temperature degassing
The mixed powder of reinforced phase and metal simple-substance or alloy is placed in vacuum or inert gas and is heated to metal simple-substance or alloy
The 50% ~ 90% of fusing point, soaking time 60min, then cools down；
(3), plate surface is handled
Sheet metal of the thickness between 0.5 ~ 3mm is chosen as jacket cladding plate, corrosion cleaning sheet metal is waited for powder green compact
Then contact surface carries out the polishing of mechanical and sand paper and completely removes surface oxide layer and exposed surface fresh metal layer, guarantees table
Surface roughness is 40 ~ 110 μm, is cleaned multiple times removal surface and oil contaminant with alcohol and acetone soln, it is to be dried after on surface to be contacted
It smears waterglass and glass lubricant is spare；
(4), powder green compact is prepared
The mixed-powder that step (2) are obtained is sent into roll and carries out powder rolling, and rolling environment temperature is 20 ~ 80 DEG C, and green compact are thick
Degree is 1 ~ 15mm；
(5), vacuum canning test specimen assembles
It is stacked according to upper cladding plate/powder green compact/lower cladding plate sequence, is surrounded by soldering and sealing plate, wherein soldering and sealing plate in two sides is provided with
Vacuum hole, preposition in vacuum heating indoor degasification in jacket welding, heating temperature is 300 DEG C, soaking time 60min, then side
Cooling side carries out the welding of vacuum edge, constitutes jacket test specimen, and will be evacuated to vacuum, vacuum degree inside jacket test specimen by vacuum hole
Are as follows: low vacuum is evacuated to: 5 × 10-1Pa, high vacuum are evacuated to: 1 × 10-2Pa carries out vacuum seal to vacuum hole after test specimen is cooling
Weldering；
(6), it rolls and is sintered
Jacket test specimen is put into the milling train for being connected to pulse current, milling train is at least made of three groups of rolls, first and last roll axis distance
Less than jacket piece lengths；The brush that can be contacted with jacket surface of test piece, pulse electricity are equipped with positioned at the two sides of upper layer roll
Flow-generator generates electric current and forms current loop through being placed in the brush of jacket surface of test piece by high-voltage output end, ground terminal, inputs
To the workshop section to be added of jacket test specimen, the on-off of current feedback circuit port and brush depends on the rolling run of jacket, and when rolling is logical
It crosses control pulse current parameter, rolling reduction ratio and rolling rate and carries out multi- pass rolling, first rolling pass reduction is not less than 13%,
Total reduction is 50% ~ 75%；
(7), sheath material cools down at room temperature, is down to 100 DEG C hereinafter, breaking jacket test specimen to temperature, taking-up pellet is made pottery
Porcelain, graphene or Carbon Fibre Reinforced Metal Matrix Composites.
2. the method that the vacuum canning rolling of impulse electric field auxiliary according to claim 1 prepares metal-base composites,
It is characterized by: each group roll of milling train is made of insulating material.
3. the method that the vacuum canning rolling of impulse electric field auxiliary according to claim 1 prepares metal-base composites,
It is characterized by: jacket specimen thickness is 0.5 ~ 3mm, length is 600 ~ 1200mm, and width is 100 ~ 300mm.
4. the method that the vacuum canning rolling of impulse electric field auxiliary according to claim 1 prepares metal-base composites,
It is characterized by: in step (6), the setting parameter of impulse current generator are as follows: 200 ~ 1000A/mm of pulse current density2, frequency
300 ~ 3000Hz of rate, 30 ~ 100 μ s of pulse width；Mill speed guarantees that powder green compact everywhere has >=5min in jacket test specimen
The discharge plasma sintering time.
5. the method that the vacuum canning rolling of impulse electric field auxiliary according to claim 2 prepares metal-base composites,
It is characterized by: the roll number of milling train is 1 ~ 5 group, each roll material is Sialon ceramics or yttria-stabilized zirconia pottery
Porcelain, mill speed are 150 ~ 500mm/min.
6. the method that the vacuum canning rolling of impulse electric field auxiliary according to claim 5 prepares metal-base composites,
It is characterized by: the roll number of milling train is n, each group brush by contact conductor can with the output end of impulse current generator and
Ground terminal connection, and with the upper surface of jacket test specimen or following table face contact, before being distributed in first group of roll, most end group roll it
Afterwards and between each group roll, respectively brush 1, brush 2 ..., brush n, successively from first group of roll to most end group roll
Distribution；Jacket test specimen front end enter at first milling train and with start rolling after first group of roll contact, when front end is contacted with brush 2
Afterwards, brush 1 and brush 2 are respectively connected to output and ground, at this time powder green compact in the jacket between brush 1 and brush 2
It is sintered；As jacket is fed, whenever front end starts to contact certain brush m(2≤m≤n) while, brush m ﹣ 1 is disconnected, and connect
Be powered brush m and ground terminal, until brush 1 and brush n are respectively connected to output and ground, has maximum sintering region at this time；
Continue to feed, brush 1 is left in jacket rear end, disconnects brush 1 and connects brush 2 and output end, at this time between brush 2 and brush n
Jacket in powder green compact be sintered, with rear end and certain brush k(k≤n ﹣ 2) separate, connection while disconnecting brush k
For brush k+1 to output end, which can guarantee that powder green compact most inside jacket test specimen is in sintering state.
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