CN102189143B - ECAE (equal channel angular extrusion) based preparation method of ultrafine crystal NiTi shape memory alloy tube - Google Patents
ECAE (equal channel angular extrusion) based preparation method of ultrafine crystal NiTi shape memory alloy tube Download PDFInfo
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- CN102189143B CN102189143B CN 201110072050 CN201110072050A CN102189143B CN 102189143 B CN102189143 B CN 102189143B CN 201110072050 CN201110072050 CN 201110072050 CN 201110072050 A CN201110072050 A CN 201110072050A CN 102189143 B CN102189143 B CN 102189143B
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Abstract
The invention provides an ECAE (equal channel angular extrusion) based preparation method of an ultrafine crystal NiTi shape memory alloy tube. A metal core is inserted into a NiTi shape memory alloy tube blank to be shaped, then the NiTi shape memory alloy tube blank is enclosed in a metal covering, and the metal covering, the NiTi shape memory alloy tube blank and the metal core are simultaneously extruded to generate shear plastic deformation in an ECAE production tool consisting of male die and a female die, so as to realize grain refinement of the NiTi shape memory alloy tube blank. Based on the fundamental of the ECAE method, a preparation method of an ultrafine crystal NiTi shape memory alloy tube is provided by the invention, so that high quality ultrafine crystal NiTi shape memory alloy tube can be produced, and production costs of the ultrafine crystal NiTi shape memory alloy tube can be reduced substantially.
Description
Technical field
What the present invention relates to is a kind of Ultra-fine Grained tubing preparation method, specifically a kind of method for preparing Ultra-fine Grained niti-shaped memorial alloy tubing based on the Equal Channel Angular Pressing technology.
Background technology
Niti-shaped memorial alloy tubing is since nineteen nineties comes out, day by day obtain people's attention in field of medical applications, especially aspect intervention inner chamber stent applications, because it can bear larger mechanical stress, has stronger radial support power, experiences larger flexural deformation and have larger resilience and the shape recovery capability, thereby shown good application prospect.Although niti-shaped memorial alloy tubing can adopt multiple manufacturing process to make, but different processing conditions can produce different impacts for the microstructure of niti-shaped memorial alloy tubing (such as the size of crystal grain, deformation texture, deformation twin etc.), thereby further SME and the load deflection mechanical behavior that affect niti-shaped memorial alloy tubing of meeting, especially suitable phase transition temperature and good super-elasticity are the important guarantees that nickel-titanium shape memory tubing is applied at biomedical sector.
Equal Channel Angular Pressing (ECAE or ECAP) technology is a kind of advanced technology that obtains super fine crystal material, this technology is the passage that equates by two axes intersect and cross sectional dimensions, machined material is extruded, made metal material produce the purpose that large shear strain realizes crystal grain thinning by the corner effect.This technology has also obtained application at present in niti-shaped memorial alloy.Document Principles of equal-channel angular pressing as a processing tool for grain refinement (Ruslan Z.Valiev, Terence G.Langdon. " Progress in Materials Science " .2006,51:881-981) with Nanostructured TiNi-based shape memory alloys processed by severe plastic deformation (V.G.Pushin, V.V.Stolyarov, R.Z.Valiev et al. " Materials Science and Engineering A " .2005,410-411:386-389), reported that two kinds of compositions (are respectively Ni
50.2Ti
49.8, Ni
50.6Ti
49.4) the ECAE technology of niti-shaped memorial alloy block materials, the grain refinement that can be with average-size after solution treatment 80 μ m is that average-size is the ultra-fine grain of 250nm, make the yield strength of alloy improve 2 times, tensile strength has improved 30%, has also significantly improved SME and the super-elasticity of niti-shaped memorial alloy.But present ECAE technology generally can only be used for preparing the block materials (circle or square-section) with ultra-fine grain, can not directly prepare the tubing with ultra-fine grain.Although be in the patent documentation of CN2690068Y at publication number, proposed a kind of device for preparing ultra-fine grain tubing, but because its device is upper with plug, fixing being difficult to of plug realized in the specific implementation, thereby to the having relatively high expectations of equipment, must carry out at the extruder of special use.And since during Equal Channel Angular Pressing inboard included angle and the outside angle ψ of mould inconsistent, the pipe tissue of a time shaping gained is inevitable inhomogeneous, must carry out multi-pass extrusion molding ability uniform formation, but because this outer surface that installs used blank is the face of cylinder, the position of each passage is difficult to accurately determine during conversion direction, therefore be difficult to guarantee to obtain uniformly tissue.In addition, intensity is high at a lower temperature, hardening capacity is strong owing to niti-shaped memorial alloy, plasticity is poor, so Equal Channel Angular Pressing having relatively high expectations to equipment of block nickel-titanium shape memory alloy material, when the Ultra-fine Grained niti-shaped memorial alloy block materials of manufacturing is used for preparing Ultra-fine Grained niti-shaped memorial alloy tubing again, production cost is greatly increased.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can prepare uniform superfine crystalline grain niti-shaped memorial alloy tubing, and can significantly reduce the Ultra-fine Grained niti-shaped memorial alloy tube preparation method based on Equal Channel Angular Pressing of the production cost of Ultra-fine Grained niti-shaped memorial alloy tubing.
The object of the present invention is achieved like this:
Inside at the niti-shaped memorial alloy pipe that will be shaped is filled in metal-cored, then the niti-shaped memorial alloy pipe is enclosed in the metallic sheath, in the ECAE frock that is formed by punch and die, to metallic sheath, niti-shaped memorial alloy pipe with metal-coredly push simultaneously, produce the shear plasticity distortion, realize the grain refinement of niti-shaped memorial alloy pipe.
The outer surface of described metallic sheath is regular polygon, metallic sheath, niti-shaped memorial alloy pipe and metal-cored finish a passage crimp after, change certain angle and carry out multi-pass crimp.
Described regular polygon is a kind of in square, regular hexagon, octagon or the dodecagon.
The invention has the advantages that:
1. the method only needs simple mould can realize directly pipe being made the tubing that interior tissue is ultra-fine grain, and the even tissue of tubing inside is consistent on common hydraulic press.
2. the rotational angle of blank when setting the jacket cross sectional shape and set every time extruding, and can accurately locating by the plane of jacket outer surface, thus realize the homogeneous deformation of whole blank, guaranteed the uniformity of pipe interior tissue.
3. by violent detrusion, can realize that niti-shaped memorial alloy tubing interior microscopic organizes the fine of grain size, greatly improve mechanical property and SME and the super-elasticity of tubing.
4. when adopting the inventive method to prepare niti-shaped memorial alloy tubing, the filling metal of pipe inside and outside jacket metal all adopt high-ductility and low intensive metal material, for the block niti-shaped memorial alloy Equal Channel Angular Pressing of difficulty distortion, can significantly reduce resistance of deformation, the niti-shaped memorial alloy pipe is in the three-dimensional compressive stress state simultaneously, be conducive to improve the plasticity of material, therefore can obtain larger distortion, and pipe be difficult for breaking.
The present invention is based on the basic principle of Equal Channel Angular Pressing, a kind of method for preparing Ultra-fine Grained niti-shaped memorial alloy tubing has been proposed, high-quality Ultra-fine Grained niti-shaped memorial alloy tubing can be produced, and the production cost of Ultra-fine Grained niti-shaped memorial alloy tubing will be significantly reduced.
Description of drawings
Fig. 1 adopts Equal Channel Angular Pressing technology jacket to prepare the basic principle schematic of ultra-fine grain niti-shaped memorial alloy tubing method.
The adoptable cross sectional shape of Fig. 2 a-Fig. 2 d metallic sheath.
Fig. 3 wrapping structure schematic diagram.
Fig. 4 extrusion process used for forming schematic diagram.
The specific embodiment
For example the present invention is done more detailed description below in conjunction with accompanying drawing:
In conjunction with Fig. 1, the basic principle for preparing ultra-fine grain niti-shaped memorial alloy tubing method based on Equal Channel Angular Pressing technology jacket of the present invention is: the inside at the niti-shaped memorial alloy pipe 4 that will be shaped fills in metal-cored 5, then it is enclosed in the metallic sheath 3, utilize ECAE frock (being formed by punch 1 and die 6) that metallic sheath 3 and inner metal pipe billet 4 and filling metal 5 thereof are carried out large shear plasticity distortion simultaneously, realize the grain refinement of niti-shaped memorial alloy pipe.Because the metal-cored and outside jacket metal of metal pipe billet inside all adopts high-ductility and low intensive metal material, for the block niti-shaped memorial alloy ECAE of difficulty distortion, can significantly reduce its resistance of deformation, the niti-shaped memorial alloy pipe is in the three-dimensional compressive stress state simultaneously, be conducive to improve the plasticity of material, therefore can obtain larger distortion, and pipe is difficult for breaking.
By ultra-fine grain niti-shaped memorial alloy tubing preparation principle figure shown in Figure 1 as can be known, because inboard included angle and the outside angle ψ of mould are inconsistent during Equal Channel Angular Pressing, can cause that suffered shearing force size is inhomogeneous everywhere, thereby so that the blank tissue odds of an extrusion molding gained is even.Therefore, in order to obtain to have the tubing of uniform superfine crystalline grain, blank must be changed certain angle and carry out multi-pass crimp.In order accurately to locate the angle that blank is changed, the employing Equal Channel Angular Pressing technology jacket that the present invention proposes prepares the cross sectional shape (shown in Fig. 2 a-Fig. 2 d) that the used jacket of ultra-fine grain niti-shaped memorial alloy tubing method can adopt multiple regular polygon, the concrete jacket of selecting which kind of cross section, to determine according to the degree of refinement of material grains, such as the less passage of need, can select square or regular hexagonal section, such as need than multi-pass, can select octagon or dodecagon cross section, can make so the more multiple location of pipe obtain maximum shear strain, thereby realize the even refinement of crystal grain.
Specific implementation process of the present invention is divided into three phases, i.e. preparatory stage, deformation stage and go the material stage.
Preparatory stage: in conjunction with figure, the cross sectional shape that at first ready sheath material is processed into as shown in Figure 2 (is got wherein a kind of, decide on arts demand, here take square sectional as example), then in blind hole identical with niti-shaped memorial alloy pipe 4 external diameter nominal sizes to be prepared of its place, axle center processing, the assurance pipe can be put in the hole, and hole depth will exceed the height of niti-shaped memorial alloy pipe 4, reserves one section space and is used for dosing metal plug 2; Then the outer surface in the niti-shaped memorial alloy pipe 4 that processes and metal-cored 5 all applies the last layer metal material, preventing because each layer intermetallic generation seam affects the niti-shaped memorial alloy pipe with the later separation work of jacket metal and core metal, and fill in the pipe 4 metal-cored 5; Again populated metal-cored 5 pipe 4 is put into metallic sheath 3; Block with the aperture of metal plug 5 with metallic sheath 3 upper ends at last.
Deformation stage: in conjunction with Fig. 4, the composite blank for preparing is put into the hole of die, mould and the blank integral body that will be fixed on the hydraulic press by heater are heated to uniform temperature and are incubated certain hour, then start hydraulic press and carry out the extrusion molding first time, after extrusion molding finishes for the first time, note blank which face up, and carry out mark; Then the hole of putting into again die behind this blank half-twist is carried out the extruding second time, also will carry out mark after the end that is shaped; Finish the 3rd, the 4th time of back extruding with same method again, even four faces of blank all carry out crimp towards the last time.
The discharging stage: after extrusion process used for forming is finished, adopt proper method that metallic sheath 3 is cut open, and take out from pipe metal-cored 5.
So just finished the preparation process of whole Ultra-fine Grained niti-shaped memorial alloy pipe.
Claims (2)
1. Ultra-fine Grained niti-shaped memorial alloy tube preparation method based on Equal Channel Angular Pressing, it is characterized in that: the inside at the niti-shaped memorial alloy pipe that will be shaped is filled in metal-cored, then the niti-shaped memorial alloy pipe is enclosed in the metallic sheath, in the ECAE frock that is formed by punch and die, to metallic sheath, niti-shaped memorial alloy pipe with metal-coredly push simultaneously, produce the shear plasticity distortion, realize the grain refinement of niti-shaped memorial alloy pipe; The outer surface of described metallic sheath is regular polygon, metallic sheath, niti-shaped memorial alloy pipe and metal-cored finish a passage crimp after, change certain angle and carry out multi-pass crimp.
2. the Ultra-fine Grained niti-shaped memorial alloy tube preparation method based on Equal Channel Angular Pressing according to claim 1 is characterized in that: described regular polygon is a kind of in square, regular hexagon, octagon or the dodecagon.
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| CN102743233A (en) * | 2012-07-24 | 2012-10-24 | 哈尔滨工程大学 | Ultra-fine grained nickel-titanium alloy root canal file and preparation method thereof |
| CN103014576A (en) * | 2013-01-05 | 2013-04-03 | 江苏大学 | Tissue superfining and anode oxidation based method for improving biomedical performance of TiNi alloy |
| CN103639218B (en) * | 2013-12-02 | 2015-06-24 | 浙江海洋学院 | Semi-automatic isometric angle extrusion testing device |
| CN103639215B (en) * | 2013-12-06 | 2016-01-06 | 山东建筑大学 | A kind of preparation method of high-strength nanocrystalline copper pipe |
| CN104897485B (en) * | 2015-03-19 | 2017-07-28 | 绍兴文理学院 | The multi-angle converting system of comprehensive structural plane tilting shearing tester |
| CN108723110B (en) * | 2017-04-19 | 2019-09-20 | 江苏华晨气缸套股份有限公司 | A method of pipeline assembly is made using marmem |
| CN107442592B (en) * | 2017-07-28 | 2019-02-12 | 江苏大学 | One kind is integrated to be squeezed and the isometrical big strain mold of corner shearing deformation of Bc mode |
| CN108480641A (en) * | 2018-03-09 | 2018-09-04 | 张家港立志传导新材料有限公司 | A kind of method that metal powder block prepares super fine crystal material |
| CN110328250B (en) * | 2019-05-10 | 2020-06-02 | 燕山大学 | Equal-channel angular extrusion processing method for pipes |
| CN111545586A (en) * | 2020-05-19 | 2020-08-18 | 燕山大学 | Equal-channel extrusion forming hydraulic machine for pipes |
| CN113426845A (en) * | 2021-07-07 | 2021-09-24 | 西北工业大学 | Extrusion method of shape memory alloy material and equal-channel angular extrusion die |
| CN114011898B (en) * | 2021-11-03 | 2023-10-20 | 中北大学 | Method for preparing superfine crystal tube by shearing, torsion and extrusion deformation |
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| CN2690068Y (en) * | 2003-06-21 | 2005-04-06 | 大连理工大学 | Device for preparing super fine grain crystal pipe by equal passage corner extrusion |
| CN2714189Y (en) * | 2004-07-19 | 2005-08-03 | 钢铁研究总院 | Equal diameter angular extrusion deformation die |
| CN201648497U (en) * | 2010-02-10 | 2010-11-24 | 江苏科技大学 | Crossed isometric angle extruding mold for preparing superfine crystal materials |
| CN101956051A (en) * | 2010-08-27 | 2011-01-26 | 武汉理工大学 | Grain refinement method and device thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7191630B2 (en) * | 2003-07-25 | 2007-03-20 | Engineered Performance Materials Co., Llc | Method and apparatus for equal channel angular extrusion of flat billets |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2690068Y (en) * | 2003-06-21 | 2005-04-06 | 大连理工大学 | Device for preparing super fine grain crystal pipe by equal passage corner extrusion |
| CN2714189Y (en) * | 2004-07-19 | 2005-08-03 | 钢铁研究总院 | Equal diameter angular extrusion deformation die |
| CN201648497U (en) * | 2010-02-10 | 2010-11-24 | 江苏科技大学 | Crossed isometric angle extruding mold for preparing superfine crystal materials |
| CN101956051A (en) * | 2010-08-27 | 2011-01-26 | 武汉理工大学 | Grain refinement method and device thereof |
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