CN1666812A - Solid stirring material preparation and modification method - Google Patents
Solid stirring material preparation and modification method Download PDFInfo
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- CN1666812A CN1666812A CN 200410003437 CN200410003437A CN1666812A CN 1666812 A CN1666812 A CN 1666812A CN 200410003437 CN200410003437 CN 200410003437 CN 200410003437 A CN200410003437 A CN 200410003437A CN 1666812 A CN1666812 A CN 1666812A
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Abstract
The invention relates to the preparation of solid agitating material and the modifying method, which uses the frictional head to rub fast the block materials, the heat of the friction maintains the raw materials in the frictional area in thermalplastification state, and uses the high-speed rotary agitating needle to misshape the thermalplastificated raw materials along with the crushing and thinning of the crystals, and meanwhile the crushed raw materials continuously turns over and mix repeatedly under the function of agitating head; during the agitating process, the agitating head moves along certain direction at proper speed. Through many times of agitating, the place that the agitating head passes through can prepare the block alloys, multiple materials or change the characters of the raw materials. The invention has simple technique, high efficiency, low cost and non-environmental pollution.
Description
Technical field
The present invention relates to the method that a kind of block materials preparation and method of modifying, particularly employing friction stirring technique prepare block alloy material, matrix material, nano material, non-crystalline material, other nonequilibrium state material and make the modification of block starting material.
Background technology
The mechanical alloying technology is proposed by the Benjamin of the U.S. the earliest, and successfully adopts this technology to prepare oxide-dispersed alloy.Its primary process is that different powder are carried out ball milling in high energy ball mill with principle, powder is under continuous collision, extruding and the impact of abrading-ball, constantly repeatedly produce distortion, fracture and seam, by interatomic phase mutual diffusion or the synthetic new powdered alloy of solid state reaction.Powder particle produces a large amount of unsalted surfaces in continuous distortion and breaking-down process, quickened solid phase diffusion or solid-phase reaction velocity.In recent decades, this technology has had very big development, can be used to produce matrix material, noncrystal and Nanoalloy powder and nonequilibrium state material.
It should be noted that: the prepared the finished product of above-mentioned mechanical alloying technology all are powder, must be by compacting, sintering or other fixed means moulding of powder, and prepare then or be processed into net shape products, and the ball milling machinery alloying technology cycle is long.People such as T.Aizawa have proposed bulk mechanical alloying (BulkMechanical Alloying, BMA) technology, make powder repeated deformation in the mould until alloying takes place by periodic external load effect (at a certain temperature), make alloy powder fixed simultaneously.Though this technology can prepare alloy cube matherial, the raw material that uses still is powder, and bulk is by sinter molding, and therefore the product of preparation can not be fine and close fully.People such as T.Ishikawa utilize aluminium foil and copper powder, magnesium powder to prepare to have superplastic aluminium alloy, though used aluminium foil as raw material, the product of alloying still is a powdered alloy.Therefore, there is following several problem in traditional mechanical alloying technology:
(1) net shape products is a powdered alloy, generally must be by other consolidation method, just can obtain block materials as the compacting of powder metallurgy and sintering etc.;
(2) be easy to generate splashing of powder, work under bad environment, contaminate environment;
(3) use powder raw material, not only cost is higher, and particle surface has impurity such as oxide compound, is difficult to prepare highly purified alloy material;
(4) need vacuum or protection of inert gas, increased the technology cost;
(5) process cycle is long.
Summary of the invention
The problem that technology of the present invention solves is: overcome the deficiencies in the prior art, provide a kind of and need not suppress and the solid-state stirring preparation method of preparation block alloy, matrix material, nano material, non-crystalline material and other nonequilibrium state material of follow-up molding procedure such as sintering and the method for modifying of material.This method has that technology is simple, efficient, cost is low, save energy, characteristics such as pollution-free, has environment-friendly function.
Technical solution of the present invention is: solid-state stirring material preparation and method of modifying, it is characterized in that: utilize the friction stir effect of machinery, the solid-state material of stirring area is fully mixed, realize the preparation and the modification of material, its concrete steps are: accompany the block materials of powdered material as raw material with block materials or centre, under certain stirring pressure effect, stirring-head is being rotated in the material material that is inserted into the needs stirring, stirring-head advances with stirring velocity and the squeeze pressure extruding set in the high speed rotating whipping process; When stirring-head moves to the appropriate location, change the direction of extrusion or the sense of rotation of stirring-head, stirring-head is back moved along former stirring trace, after repeatedly repeating stirring action, prepare required alloy material, matrix material or make the starting material modification in the inswept zone of stirring-head; The finished product of preparation still are solid-state block materials.
Described block materials is metal alloy compositions, non-metallic material, matrix material, nano material, non-crystalline material or other nonequilibrium state material.
The speed of rotation of described stirring-head is 100-4000 rev/min, stir translational speed and be 0.01-30 rice/minute, stirring pressure is 0.1-200MPa, squeeze pressure is 0.1-150MPa.
Described metal alloy compositions is for being base with a kind of metal, adding the alloy material of one or more alloying elements formation; Non-metallic material are macromolecular material or ceramic; Matrix material is a metal-base composites, or ceramic matric composite, or polymer-based composite; Nano material is that grain-size has the block materials less than 100 nanometer scale; Non-crystalline material is the amorphous metal block materials; The nonequilibrium state material is the block materials that composition over balance phasor is limited.
Principle of the present invention is: by stirring-head to the quick friction of bulk raw material, stir the heat that is produced, make the starting material of friction area be in the thermoplasticity state, mixing needle by high speed rotating makes the starting material that are in the thermoplasticity state that big viscous deformation take place, and while crystal grain is broken, refinement.Broken starting material constantly roll up and down, repeat to mix under the effect of stirring-head.Stirring-head pushes forward along certain specific direction with certain speed in the high speed rotating whipping process, when stirring-head moves to the appropriate location, changes the direction of extrusion or the sense of rotation of stirring-head, and stirring-head is back moved along former stirring trace.Behind repetition stirring action repeatedly, can prepare required material or make material modification in the inswept zone of stirring-head.Owing to can fully contact between the different starting material constituent elements in the whipping process, there is the interface of cleaning fully between the variable grain, the heat that friction is simultaneously produced raises material temperature, further improve velocity of diffusion, reach the purpose of accelerated material interfacial diffusion or solid state reaction, so this technology can be used as a kind of mechanical alloying technology and the method for preparing matrix material.Simultaneously, the crystal grain of original position is broken and big viscous deformation takes place in the starting material, can change raw-material performance, so this technology also can be used as a kind of method of material modification.Through constantly stir fast, broken and cooling fast, can make grain-size in the material less than 100 μ m, therefore can prepare the nanometer bulk; Further stir and cooling, can prepare non-crystalline material.
The advantage that the present invention compared with prior art has is as follows:
(1) with block materials (can add the part powder places between the bulk as interlayer) as raw material, avoided the dust in the material preparation process to splash; In preparation process, do not need vacuum condition and gas shield; Owing to liquid can not occur in the solid-state whipping process, not have gas to produce yet; Therefore, this technology has not only been saved the technology cost, still a kind of free of contamination Environmentally-sound technology;
(2) by the high speed rotating of stirring-head and certain pressure effect, can prepare bulk alloy, matrix material, nano material, non-crystalline material and other nonequilibrium state material, promptly Zhi Bei net shape products is the solid bulk, can directly carry out follow-up press working or hot-work, need compacting and sintering or bonding; Therefore, compare with traditional mechanical alloying technology, this technology has not only been simplified the operation of preparation material, reduces preparation cost, the more important thing is to obtain fine and close fully bulk material, and the performance of product can be further enhanced;
(3) the compoundization process of alloying or material is carried out in block materials inside, can avoid the oxidation of material and the introducing of impurity, is beneficial to highly purified alloy of preparation or matrix material;
(4) the heat of friction overwhelming majority between stirring-head and the raw material is converted into the required energy of material preparation; Therefore this technology has the characteristics of save energy, and process cycle is short;
(5) working condition of this technical requirements is loose, and equipment is simple, is beneficial to the realization automatic production, can enhance productivity.
Description of drawings
Fig. 1 is the solid-state stirring material preparation method of a present invention principle schematic;
Fig. 2 is solid-state stirring material preparation of the present invention or method of modifying principle schematic;
Fig. 3 prepares the solid-state stirring alloying technology process of alloy for the embodiment of the invention 1 adopts laminated material;
Fig. 4 prepares the solid-state stirring alloying technology process of alloy for the embodiment of the invention 2 adopts laminated material;
Fig. 5 adopts the distributing mode of laminated material and powdered preparation alloy for the present invention;
Solid-state stirring material preparation and modified device structural representation that Fig. 6 adopts for the present invention.
Embodiment
Embodiment 1, as shown in Figure 1, 2, utilizes solid-state stirring material preparation and modified device shown in Figure 6 to prepare the magnesium-aluminum alloy material.Starting material A, B are respectively pure magnesium and fine aluminium.Equipment is made up of stirring-head 1, drive system 2, worktable 3, Controlling System 4 and pressure system 5.The action of entire equipment is by Controlling System 4 controls, and worktable 3 is used for fixing sample, and pressure system 5 provides stirring pressure and worktable 3 required in stirring-head 1 working process to move required squeeze pressure; The running fix of the speed of rotation of stirring-head 1, downstream rate and worktable 3 is by drive system 2 controls of system.
Concrete preparation process is:
(1) starting material magnesium, aluminium plate is stacked alternately together, shown in Fig. 3 a;
(2) laminated material is fixed on the worktable 3, shown in Fig. 3 b;
(3) mixing needle of stirring-head 1 is being rotated along stack direction or with in certain angle (＜90 °) insertion laminated material, shown in Fig. 3 c;
(4) adjust operating device 4 and make stirring-head 1, drive worktable 3 simultaneously and push forward along certain orientation with ω=500-3000 rev/min speed rotation, translational speed V=0.1-10 rice/minute, stir pressure P=40-200MPa, shown in Fig. 3 d;
When (5) stirring-head 1 moves to the position that sets, change the sense of rotation of stirring-head 1, toward reverse direction traverser 3, repeat above-mentioned (4) process again, till obtaining required magnesium-aluminum alloy.
Embodiment 2, and as shown in Figure 4, the ma process for preparing magnesium-aluminum alloy with pure magnesium A of starting material and fine aluminium B is:
(1) magnesium, aluminium are stacked alternately together, shown in Fig. 4 a;
(2) laminated material magnesium and aluminium are fixed on the worktable 3, shown in Fig. 4 b;
(3) mixing needle of stirring-head is being rotated along in the interface direction insertion laminated material of lamination, shown in Fig. 4 c;
(4) make the stirring-head high speed rotating, rotating speed is ω=500-3000 rev/min, and moves along lamination interface direction, the mixing needle translational speed be V=0.1-10 rice/minute, stir pressure P=40-200MPa, shown in Fig. 4 d;
(5) move stirring-head toward reverse direction, repetitive process (4) is till obtaining required magnesium-aluminum alloy.
Embodiment 3, and the mechanical alloy for preparing magnesium-aluminum alloy with pure magnesium sheet material and aluminium powder form turns to example, and its distributing mode is shown in Figure 5, and technological process is with embodiment 1 or embodiment 2.
Embodiment 4, are example to prepare polymer composite by two kinds of different polymer sheet materials, and its technological process is with embodiment 1 or embodiment 2.Wherein, ω=100-1000 rev/min of stirring-head speed of rotation, mixing needle translational speed be V=1-10 rice/minute, stir pressure P=0.1-40MPa.
Embodiment 5, with sheet metal with second mutually the granules preparation particles reiforced metal-base composition be example, its distributing mode as shown in Figure 5, technological process is with embodiment 1 or embodiment 2.
Embodiment 6, and preparing ptc material with polyethylene board and carbon black pellet is example, its distributing mode as shown in Figure 5, technological process is with embodiment 1 or embodiment 2.Wherein, ω=100-1000 rev/min of stirring-head speed of rotation, mixing needle translational speed be V=1-10 rice/minute, stir pressure P=0.1-40MPa.
Embodiment 7, and preparing the copper nano material with the metallic copper bulk is example.Its technological process is:
(1) is fixed on the copper billet material on the worktable 3 and places water or oil;
(2) all the other technological processs are with embodiment 1 or embodiment 2.
Embodiment 8, and preparing the copper non-crystalline material with the metallic copper bulk is example.Its technological process is with embodiment 7.
Embodiment 9, prepare by immiscible aluminium, the plumbous nonequilibrium state material of forming with metallic aluminium sheet material and stereotype material.Its technological process is:
(1) presses the material composition design requirements, choose metallic aluminium, the stereotype material of certain thickness ratio, raw material is stacked together by the distributing mode shown in Fig. 3 a;
(2) technological process is with embodiment 1 or embodiment 2.
Embodiment 10, are example with the grain refining of metallic aluminium upper layer.Its technological process is:
(1) the metal aluminium is fixed on the worktable 3;
(2) mixing needle of stirring-head 1 is being rotated in the insertion metallic aluminium, shown in Fig. 4 c;
(3) make the stirring-head high speed rotating, rotating speed is ω=500-3000 rev/min, and moves along certain direction of metallic aluminium surface, the mixing needle translational speed be V=0.1-10 rice/minute, shown in Fig. 4 d;
(4) move stirring-head toward reverse direction, repetitive process (3) is till the aluminium upper layer that obtains required grain-size.
Claims (13)
1, solid-state stirring material preparation and method of modifying, it is characterized in that: utilize the friction stir effect of machinery, the solid-state material of stirring area is fully mixed, prepare new material or make the starting material modification, the steps include: to accompany the block materials of powder as raw material with block materials or centre, under certain stirring pressure effect, stirring-head is being rotated in the material that is inserted into the needs stirring, stirring-head advances with stirring velocity and the squeeze pressure extruding set in the high speed rotating whipping process; When stirring-head moves to the appropriate location, change the direction of extrusion or the sense of rotation of stirring-head, stirring-head is back moved along former stirring trace; After repeatedly repeating stirring action, can prepare required solid-state block product or make the starting material modification in the inswept zone of stirring-head, the finished product of preparation still are solid-state block materials.
2, solid-state stirring material preparation according to claim 1 and method of modifying, it is characterized in that: described block starting material are pure metal or metal alloy compositions or non-metallic material or matrix material.
3, solid-state stirring material preparation according to claim 1 and method of modifying, it is characterized in that: described final solid-state block product is pure metal or metal alloy compositions or non-metallic material or matrix material or nano material or non-crystalline material, or other nonequilibrium state material.
4, solid-state stirring material preparation according to claim 1 and method of modifying, it is characterized in that: the speed of rotation of described stirring-head is 200-4000 rev/min.
5, solid-state stirring material preparation according to claim 1 and method of modifying is characterized in that: described stirring-head translational speed be 0.01-30 rice/minute.
6, solid-state stirring material preparation according to claim 1 and method of modifying, it is characterized in that: described stirring pressure is 0.1-200MPa.
7, solid-state stirring material preparation according to claim 1 and method of modifying, it is characterized in that: described squeeze pressure is 0.1-150MPa.
8, according to claim 2 or 3 described solid-state stirring materials preparation and method of modifying, it is characterized in that: described metal alloy compositions is for being base with a kind of metal, adding the alloy material of one or more alloying elements formation.
9, according to claim 2 or 3 described solid-state stirring material preparation and method of modifying, it is characterized in that: described non-metallic material are macromolecular material or ceramic.
10, according to claim 2 or 3 described solid-state stirring material preparation and method of modifying, it is characterized in that: described matrix material is a metal-base composites, or ceramic matric composite, or polymer-based composite.
11, according to claim 2 or 3 described solid-state stirring material preparation and method of modifying, it is characterized in that: described nano material is that grain-size has the block materials less than 100 nanometer scale.
12, according to claim 2 or 3 described solid-state stirring material preparation and method of modifying, it is characterized in that: described non-crystalline material is the amorphous metal block materials.
13, according to claim 2 or 3 described solid-state stirring material preparation and method of modifying, it is characterized in that: described nonequilibrium state material is the block materials that composition over balance phasor is limited.
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| CN 200410003437 CN1666812A (en) | 2004-03-10 | 2004-03-10 | Solid stirring material preparation and modification method |
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| CN 200410003437 CN1666812A (en) | 2004-03-10 | 2004-03-10 | Solid stirring material preparation and modification method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820662A (en) * | 2014-02-28 | 2014-05-28 | 宝山钢铁股份有限公司 | Method of enhancing refining effect of zirconium for aluminum-free magnesium alloy casting structure |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820662A (en) * | 2014-02-28 | 2014-05-28 | 宝山钢铁股份有限公司 | Method of enhancing refining effect of zirconium for aluminum-free magnesium alloy casting structure |
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