CN106269971B - A kind of method that multidirectional compression torsion Compound Extrusion prepares micro-nano copper - Google Patents

A kind of method that multidirectional compression torsion Compound Extrusion prepares micro-nano copper Download PDF

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CN106269971B
CN106269971B CN201610676583.9A CN201610676583A CN106269971B CN 106269971 B CN106269971 B CN 106269971B CN 201610676583 A CN201610676583 A CN 201610676583A CN 106269971 B CN106269971 B CN 106269971B
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copper
micro
nano
extrusion
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CN106269971A (en
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黄树海
陈强
赵祖德
宁海青
胡传凯
夏祥生
舒大禹
王艳彬
柴舒心
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Southwest Institute of Technology and Engineering of China South Industries Group
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No 59 Research Institute of China Ordnance Industry
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Extrusion Of Metal (AREA)
  • Forging (AREA)

Abstract

The invention discloses a kind of multidirectional compression torsion Compound Extrusion method for preparing micro-nano copper, including:(1)Copper ingot base is subjected to softening pretreatment;(2)By step(1)Obtained blank carries out multidirectional compression cycle extrusion, makes blank that large plastometric set occur, crystallite dimension is refine to submicron order;(3)By step(2)Obtained blank carries out rounding processing, obtains designed blank shape size;(4)By step(3)Obtained blank carries out stress relief annealing process;(5)By step(4)Obtained blank carries out movable matrix torsion and squeezes, and makes blank that multistage forward extrusion necking down deformation occur, crystallite dimension is refine to micro/nano level;(6)By step(5)Obtained blank carries out microstructure sampling analysis, and guarantee prepares micro-nano copper structure property.Present invention could apply to the preparations of the Ultra-fine Graineds such as fine copper, brass, copper-nickel alloy and micro Nano material.

Description

A kind of method that multidirectional compression torsion Compound Extrusion prepares micro-nano copper
Technical field
The present invention relates to a kind of methods that multidirectional compression torsion Compound Extrusion prepares micro-nano copper.
Background technology
Micro-nano copper and copper alloy are the important directions of advanced material technology development.The crystal grain ruler of micro-nano copper and copper alloy It is very little ultra-fine, there are some physical properties and mechanical property for being different from conventional material.Traditional crystallite dimension refinement is mainly logical The big forging ratio deformation of excessively high finish forge equipment and high frequency forge cogging, promote die break and refinement, and crystal grain is inhibited to grow up, but crystal grain Size is typically in hundred micron orders, it is difficult to which crystallite dimension is refine to submicron order or even micro/nano level.At present, about micro-nano The preparation of rice copper and copper alloy mainly has two big methods, first, bottom-to-top method, that is, pass through physics, chemically or mechanically method It prepares ultra-fine powder, then micro-nano copper base, but the cost of this method is prepared by the methods of powder sintered, densification Higher, unavoidably there are residual porosity and powder impurity pollution effect, and the micro-nano copper specification prepared is smaller;Second is that from Method under above, i.e., directly carry out block-like copper and copper alloy severe plastic deformation processing, and such as Equal Channel Angular Pressing, accumulation is folded Roll, high pressure torsion the methods of, both at home and abroad correlation scholar fundamental research has been carried out using small sample, be prepared for micro/nano level Copper and copper alloy, but this method deformed area material hydrostatic pressure very little, mainly based on shear strain, microdefect can not be effective It is closed and repairs, the intensity of some super fine crystal materials is higher, plasticity is poor, and mostly small in micro-nano copper and copper alloy Sample preparatory phase does not obtain effective engineer application also.
Invention content
The object of the present invention is to provide a kind of methods that multidirectional compression torsion Compound Extrusion prepares micro-nano copper.
To achieve these goals, using following technical scheme.
The compound method for preparing micro-nano copper is reversed in a kind of multidirectional compression, it is characterised in that is included the following steps:
(1)Softening pretreatment:Copper and copper alloy ingot blank are subjected to furnace cooling after softening heat treatment, to blank sampling analysis Tissue and crystallite dimension state;
(2)Multidirectional compression cycle extrusion:By blank first along blank short transverse, i.e. highest is axially compressed;Then Blank is overturn 90 °, along charge length direction, i.e. highest is axially compressed;Blank is overturn 90 ° again, along blank width side To that is, highest is axially compressed;So cycle is multiple;A micronization processes to blank crystallite dimension are completed, make blank brilliant Particle size reaches submicron order;
(3)Roundingization processing:Blank shape is subjected to rotation free compression or round as a ball, promotes blank rounding;Then it carries out Enclosed jumping-up obtains designed blank shape size;
(4)Low temperature destressing is handled:Promote blank that static recovery occurs, blank tissue should during the multidirectional compression of elimination squeezes Power is concentrated, while treated that crystallite dimension is not significantly grown up for blank;
(5)Movable matrix torsion squeezes:Blank is placed in the cavity plate that can be rotated in an axial direction, blank is in punching die Effect is lower to occur certain plastic deformation, and after being adjacent to concave die cavity, while cavity plate is rotated along axis is squeezed with a fixed angular speed, Promote blank that multistage forward extrusion necking down deformation occurs, the sectional area of blank necking region is sequentially reduced, the blank of final extruding end Diameter reaches designed bar diameter, completes the secondary micronization processes to blank crystallite dimension, reaches blank crystallite dimension Micro/nano level;
(6)Microstructure sampling analysis:Analyze blank softening pretreatment state, multidirectional squeezed state, low temperature destressing state, activity Cavity plate reverses the tissue change and degree of grain refinement of As-extruded.
Step(2)Described in multidirectional compression cycle extrusion deformation temperature for room temperature, Uniaxial Compression deflection 30~ 60%, ensure that blank average grain size is less than 10 μm by sampling analysis.
Step(5)Described in movable matrix torsion squeeze and make blank that three-level necking down deformation, necking down circle diameter of bore occur Become smaller step by step, deflection reduces step by step, and necking down deflection at different levels is not less than 30%.
The upper cone angle of the necking down circle is 120 ± 5o, and lower cone angle beta is 20 ± 3o.
The cavity plate is rotated along axis is squeezed with 0.5rad/s ~ 5rad/s angular speed.
The present invention provides the preparation methods of the micro-nano copper of big specification, and Compound Extrusion technology is reversed by multidirectional compression, The Steady-State security of reinforcing material reduces the formation and extension of microdefect during drastic deformation, by hundred micron-sized copper and Copper alloy ingot blank is converted into the copper of micro/nano level and copper alloy bar stock, and it is comprehensive to improve the yield tensile ratio, ductility, dynamic jet flow of material etc. Close performance, realize by the micro-nano copper rod base of big specification be applied to high-end equipment key structure manufacture, improve its manufacture service life, It is on active service and explosion power, while manufactures that at low cost, manufacture efficiency is high, be easy to engineer application.
Figure of description
Fig. 1 is micro-nano copper preparation flow figure in the present invention;
Fig. 2 squeezes schematic diagram for movable matrix torsion;
Fig. 3 is necking down coil structures schematic diagram.
In figure, 1-punch-pin;2-movable matrix;3-first order necking down circle;4-second level necking down circle;5-third level contracts Neck ring;6-extruding axis;Blank before 7-deformation;Blank after 8-deformation;9-guide cylinder.
Specific embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1
(1)Φ 65mm fine copper bars are selected, the fine copper ingot blank of length, width and height 108mm × 65mm × 60mm is processed by forging, Then in temperature 400 DEG C made annealing treatment, cool to room temperature with the furnace after soaking time 2.0h.
(2)Manufacturing and designing length, width and height has a certain proportion of mold cavity, first along ingot blank short transverse, i.e. highest axial direction Compression is carried out, until full of cavity;Then blank is overturn 90 °, along its length, i.e., highest axially carries out jumping-up pressure Contracting, until full of cavity;Blank is overturn 90 ° again, in the width direction, i.e., highest axially carries out Compression, until full of type Chamber;So cycle extrusion 16 times, it is sampled to measure 4 μm of average grain size.
(3)After blank shape is carried out rotation free compression, enclosed jumping-up is then carried out, obtains the blank of Φ 60mm.
(4)Then by blank in 100 DEG C of progress stress relief annealing process of temperature, soaking time 40min.
(5)Manufacture and design movable matrix torsion extrusion die, blank is placed in the cavity plate that can be rotated in an axial direction, blank Certain plastic deformation occurs under the action of punching die, after being adjacent to concave die cavity, while cavity plate along squeeze axis with one Fixed angular speed rotates, and blank subsequently enters first order necking down circle, and diameter of section is decreased to Φ 42mm, subsequently enters second level necking down Circle, diameter of section are decreased to Φ 30mm, finally enter third level necking down circle, and diameter of section is decreased to Φ 24mm.
(6)It is processed to obtain the blank of Φ 24mm after blank is removed from the molds, it is sampled to measure average crystal grain ruler Very little 86nm.
Embodiment 2
(1)Φ 85mm ormolu bars are selected, are closed by the copper zinc of forging processing length, width and height 152mm × 85mm × 80mm Ingot base, then in temperature 400 DEG C made annealing treatment, cool to room temperature with the furnace after soaking time 2.0h.
(2)Manufacturing and designing length, width and height has a certain proportion of mold cavity, first along ingot blank short transverse, i.e. highest axial direction Compression is carried out, until full of cavity;Then blank is overturn 90 °, along its length, i.e., highest axially carries out jumping-up pressure Contracting, until full of cavity;Blank is overturn 90 ° again, in the width direction, i.e., highest axially carries out Compression, until full of type Chamber;So cycle extrusion 18 times, it is sampled to measure 7 μm of average grain size.
(3)After blank shape is carried out rotation free compression, enclosed jumping-up is then carried out, obtains the blank of Φ 80mm.
(4)Then by blank in 110 DEG C of progress stress relief annealing process of temperature, soaking time 30min.
(5)Manufacture and design movable matrix torsion extrusion die, blank is placed in the cavity plate that can be rotated in an axial direction, blank Certain plastic deformation occurs under the action of punching die, after being adjacent to concave die cavity, while cavity plate along squeeze axis with one Fixed angular speed rotates, and blank subsequently enters first order necking down circle, and diameter of section is decreased to Φ 56mm, subsequently enters second level necking down Circle, diameter of section are decreased to Φ 40mm, finally enter third level necking down circle, and diameter of section is decreased to Φ 30mm.
(6)It is processed to obtain the blank of Φ 30mm after blank is removed from the molds, it is sampled to measure average crystal grain ruler Very little 180nm.
Multidirectional compression torsion coextrusion method proposed by the present invention, it is multidirectional to compress in extrusion process at material major part In Steady-State security state, be conducive to improve the plasticity of material, reduce cracking defect;Movable matrix torsion, which squeezes, can change base Frotteurism between material and extrusion cylinder, advantageously reduces resistance of deformation, it is easy to accomplish the batch system of micro-nano copper and copper alloy It is standby.

Claims (3)

1. a kind of method that multidirectional compression torsion Compound Extrusion prepares micro-nano copper, it is characterised in that include the following steps:
(1)Softening pretreatment:Copper or copper alloy ingot blank are subjected to furnace cooling after softening heat treatment, to blank sampling analysis tissue And crystallite dimension state;
(2)Multidirectional compression cycle extrusion:Blank is compressed first along blank short transverse;Then blank is overturn 90 °, edge It is compressed in charge length direction;Blank is overturn 90 ° again, is compressed along blank width direction;So cycle is multiple;It completes To a micronization processes of blank crystallite dimension, blank crystallite dimension is made to reach submicron order;
(3)Roundingization processing:Blank shape is subjected to rotation free compression or round as a ball, promotes blank rounding;Then enclosed is carried out Jumping-up obtains designed blank shape size;
(4)Low temperature destressing is handled:Promote blank that static recovery occurs, eliminate the stress collection of blank tissue during multidirectional compression squeezes In;
(5)Movable matrix torsion squeezes:Blank is placed in the cavity plate that can be rotated in an axial direction, blank is in the effect of punching die Lower that certain plastic deformation occurs, after being adjacent to concave die cavity, while cavity plate is rotated along axis is squeezed, and blank is promoted to occur multistage Forward extrusion necking down deforms, and the sectional area of blank necking region is sequentially reduced, and the blank diameter of final extruding end reaches designed Bar diameter completes the secondary micronization processes to blank crystallite dimension, blank crystallite dimension is made to reach micro/nano level;
(6)Microstructure sampling analysis:Analyze blank softening pretreatment state, multidirectional squeezed state, low temperature destressing state, movable matrix Reverse the tissue change and degree of grain refinement of As-extruded;
Step(5)Described in movable matrix torsion squeeze and make blank that three-level necking down deformation occur, necking down circle diameter of bore is step by step Become smaller, deflection reduces step by step, and necking down deflection at different levels is not less than 30%;
The upper cone angle of the necking down circle is 120 ± 5o, and lower cone angle beta is 20 ± 3o.
2. the method that multidirectional compression torsion Compound Extrusion as described in claim 1 prepares micro-nano copper, it is characterised in that step (2)Described in multidirectional compression cycle extrusion deformation temperature for room temperature, Uniaxial Compression deflection 30~60% passes through sampling point Analysis ensures that blank average grain size is less than 10 μm.
3. the method that multidirectional compression torsion Compound Extrusion as described in claim 1 prepares micro-nano copper, the cavity plate is along crowded Last item is rotated with 0.5rad/s ~ 5rad/s angular speed.
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CN102002656A (en) * 2010-11-10 2011-04-06 中南大学 Method for refining separated or dispersion-strengthening type block copper alloy crystal particles
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JP2005000993A (en) * 2003-05-16 2005-01-06 Susumu Mizunuma Non-axial symmetric twist-extruding method for material
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CN101509116A (en) * 2008-05-12 2009-08-19 昆明理工大学 Method for producing ultra-fine grain by using repeated forging of large deformation
CN102002656A (en) * 2010-11-10 2011-04-06 中南大学 Method for refining separated or dispersion-strengthening type block copper alloy crystal particles
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