CN106269971A - The method that Compound Extrusion prepares micro-nano copper is reversed in a kind of multidirectional compression - Google Patents
The method that Compound Extrusion prepares micro-nano copper is reversed in a kind of multidirectional compression Download PDFInfo
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- CN106269971A CN106269971A CN201610676583.9A CN201610676583A CN106269971A CN 106269971 A CN106269971 A CN 106269971A CN 201610676583 A CN201610676583 A CN 201610676583A CN 106269971 A CN106269971 A CN 106269971A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 230000006835 compression Effects 0.000 title claims abstract description 31
- 238000007906 compression Methods 0.000 title claims abstract description 31
- 239000010949 copper Substances 0.000 title claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 29
- 238000001125 extrusion Methods 0.000 title claims abstract description 29
- 150000001875 compounds Chemical class 0.000 title claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 230000002441 reversible effect Effects 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 5
- 239000000523 sample Substances 0.000 claims description 5
- 239000012496 blank sample Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 230000002829 reductive effect Effects 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims 1
- 238000000137 annealing Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- 229910000570 Cupronickel Inorganic materials 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000000956 alloy Substances 0.000 abstract 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 abstract 1
- 229910052683 pyrite Inorganic materials 0.000 abstract 1
- 239000011028 pyrite Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000003247 decreasing effect Effects 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 206010017389 Frotteurism Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- -1 has two big methods Chemical compound 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture 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 and reverse the method that Compound Extrusion prepares micro-nano copper, including: copper ingot base is carried out softening pretreatment by (1)；(2) blank that step (1) obtains is carried out multidirectional compression cycle extrusion, make blank generation large plastometric set, crystallite dimension is refine to submicron order；(3) blank that step (2) obtains is carried out rounding process, obtain designed blank shape size；(4) blank that step (3) obtains is carried out stress relief annealing process；(5) blank that step (4) obtains is carried out movable matrix and reverses extruding, make blank that multistage forward extrusion necking down deformation to occur, crystallite dimension is refine to micro/nano level；(6) blank that step (5) obtains is carried out microstructure sample analysis, it is ensured that prepare micro-nano copper structure property.Present invention could apply to Ultra-fine Grained and the preparations of micro Nano material such as fine copper, pyrite, copper-nickel alloy.
Description
Technical field
The present invention relates to a kind of multidirectional compression and reverse the method that 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 chi of micro-nano copper and copper alloy
Very little ultra-fine, there are some physical property being different from conventional material and mechanical properties.Traditional crystallite dimension refinement is the most logical
The big forging ratio deformation of too high finish forge equipment and high frequency forge cogging, promote die break and refinement, inhibiting grain growth, but crystal grain
Size is typically in hundred micron orders, is difficult to crystallite dimension is refine to submicron order, even micro/nano level.Currently, with respect to micro-nano
The preparation of rice copper and copper alloy mainly has two big methods, and one is bottom-to-top method, i.e. by physics, chemically or mechanically method
Prepare ultra-fine powder body, then prepare micro-nano copper base by methods such as powder sintered, densification, but the cost of the method
Higher, unavoidably there is residual porosity and powder impurity pollution effect, and the micro-nano copper specification prepared is less；Two is certainly
Upper and lower method, i.e. directly carries out severe plastic deformation processing to block copper and copper alloy, as Equal Channel Angular Pressing, accumulation are folded
Roll, the method such as high pressure torsion, the most relevant scholar uses small sample to carry out fundamental research, is prepared for micro/nano level
Copper and copper alloy, but the method deformed area material hydrostatic pressure is the least, and mainly based on shear strain, microdefect cannot be effective
Guan Bi and repairing, the intensity of some super fine crystal materials is higher, plasticity is poor, and is mostly in the little of micro-nano copper and copper alloy
Sample preparatory phase, does not also obtain effective engineer applied.
Summary of the invention
It is an object of the invention to provide a kind of multidirectional compression and reverse the method that Compound Extrusion prepares micro-nano copper.
To achieve these goals, by the following technical solutions.
The compound method preparing micro-nano copper is reversed in a kind of multidirectional compression, it is characterised in that comprise the steps:
(1) pretreatment is softened: carry out copper and copper alloy ingot blank softening furnace cooling after heat treatment, to blank sample analysis tissue
And crystallite dimension state；
(2) multidirectional compression cycle extrusion: by blank first along blank short transverse, the highest is axially compressed；Then by base
Material upset 90 °, along charge length direction, the highest is axially compressed；Again blank is overturn 90 °, along blank width direction, i.e.
The highest axially it is compressed；So circulation is repeatedly；Complete a micronization processes to blank crystallite dimension, make blank crystallite dimension
Reach submicron order；
(3) roundingization processes: carries out blank shape rotating 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 processes: promote blank generation static recovery, eliminates the stress collection of blank tissue in multidirectional compression extruding
In, the crystallite dimension after blank processes simultaneously is the most substantially grown up；
(5) movable matrix reverses extruding: being placed in by blank in the die that can rotate vertically, blank is in the effect of upper mold drift
The plastic deformation that lower generation is certain, after being adjacent to concave die cavity, die rotates along extrusion axis with a fixed angular speed simultaneously, promotes
There is multistage forward extrusion necking down deformation in blank, the sectional area of blank necking region is sequentially reduced, the blank diameter of final extruding end
Reach designed bar diameter, complete the secondary micronization processes to blank crystallite dimension, make blank crystallite dimension reach micro-nano
Meter level；
(6) microstructure sample analysis: analyze blank and soften pretreatment state, multidirectional squeezed state, low temperature destressing state, movable matrix
Reverse tissue change and the degree of grain refinement of As-extruded.
The deformation temperature of the multidirectional compression cycle extrusion described in step (2) is room temperature, Uniaxial Compression deflection 30～
60%, guarantee that blank average grain size is less than 10 μm by sample analysis.
Movable matrix described in step (5) reverses extruding makes blank that three grades of necking down deformation, necking down circle diameter of bore to occur
Diminishing 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 described necking down circle is 120 ± 5, and lower cone angle beta is 20 ± 3.
Described die rotates along extrusion axis with 0.5rad/s ~ 5rad/s angular velocity.
The invention provides the preparation method of the micro-nano copper of big specification, reverse Compound Extrusion technology by multidirectional compression,
The Steady-State security of reinforcing material, reduces formation and the extension of microdefect during drastic deformation, by hundred micron-sized copper and
Copper alloy ingot blank is converted into copper and the Copper alloy bar base of micro/nano level, improves the yield tensile ratio of material, ductility, dynamic jet flow etc. and combines
Close performance, it is achieved the micro-nano copper rod base of big specification is applied to the manufacture of high-end equipment key structure, improve its manufacture life-span,
It is on active service and explosion power, is simultaneously fabricated into low, a manufacture efficiency height, it is easy to engineer applied.
Figure of description
Fig. 1 be in the present invention micro-nano copper for flow chart；
Fig. 2 is that movable matrix reverses extruding schematic diagram；
Fig. 3 is necking down coil structures schematic diagram.
In figure, 1 punch；2 movable matrixes；3 first order necking down circles；4 second level necking down circles；5 third level contractings
Neck ring；6 extrusion axises；Blank before 7 deformation；Blank after 8 deformation；9 guide cylinders.
Detailed description of the invention
Below in conjunction with example, the invention will be further described.
Embodiment 1
(1) Φ 65mm fine copper bar is selected, through the fine copper ingot blank of forging processing length, width and height 108mm × 65mm × 60mm, then
Make annealing treatment temperature 400 DEG C, after temperature retention time 2.0h, cool to room temperature with the furnace.
(2) manufacture and design length, width and height and there is a certain proportion of mold cavity, first along ingot blank short transverse, the highest axially
Carry out Compression, until being full of die cavity；Then blank is overturn 90 °, along its length, the highest axially carry out jumping-up pressure
Contracting, until being full of die cavity；Again blank is overturn 90 °, in the width direction, the highest axially carry out Compression, until being full of type
Chamber；So cycle extrusion 16 times, sampled records average grain size 4 μm.
(3), after carrying out blank shape rotating free compression, then carry out enclosed jumping-up, obtain the blank of Φ 60mm.
(4) then temperature 100 DEG C, blank being carried out stress relief annealing process, temperature retention time is 40min.
(5) manufacture and design movable matrix and reverse extrusion die, blank is placed in the die that can rotate vertically, blank
Under the effect of upper mold drift, there is certain plastic deformation, after being adjacent to concave die cavity, simultaneously die along extrusion 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 is decreased to Φ 30mm, finally enters third level necking down circle, and diameter of section is decreased to Φ 24mm.
(6) it is processed obtaining the blank of Φ 24mm after being removed from the molds by blank, sampled records average crystal grain chi
Very little 86nm.
Embodiment 2
(1) Φ 85mm ormolu bar is selected, through the ormolu ingot of forging processing length, width and height 152mm × 85mm × 80mm
Base, then makes annealing treatment temperature 400 DEG C, cools to room temperature after temperature retention time 2.0h with the furnace.
(2) manufacture and design length, width and height and there is a certain proportion of mold cavity, first along ingot blank short transverse, the highest axially
Carry out Compression, until being full of die cavity；Then blank is overturn 90 °, along its length, the highest axially carry out jumping-up pressure
Contracting, until being full of die cavity；Again blank is overturn 90 °, in the width direction, the highest axially carry out Compression, until being full of type
Chamber；So cycle extrusion 18 times, sampled records average grain size 7 μm.
(3), after carrying out blank shape rotating free compression, then carry out enclosed jumping-up, obtain the blank of Φ 80mm.
(4) then temperature 110 DEG C, blank being carried out stress relief annealing process, temperature retention time is 30min.
(5) manufacture and design movable matrix and reverse extrusion die, blank is placed in the die that can rotate vertically, blank
Under the effect of upper mold drift, there is certain plastic deformation, after being adjacent to concave die cavity, simultaneously die along extrusion 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 is decreased to Φ 40mm, finally enters third level necking down circle, and diameter of section is decreased to Φ 30mm.
(6) it is processed obtaining the blank of Φ 30mm after being removed from the molds by blank, sampled records average crystal grain chi
Very little 180nm.
The multidirectional compression that the present invention proposes reverses coextrusion method, in its multidirectional compression extrusion process at material major part
In Steady-State security state, be conducive to improving the plasticity of material, reduce cracking defect；Movable matrix reverses extruding can change base
Frotteurism between material and recipient, advantageously reduces resistance of deformation, it is easy to accomplish micro-nano copper and the batch system of copper alloy
Standby.
Claims (5)
1. the compound method preparing micro-nano copper is reversed in a multidirectional compression, it is characterised in that comprise the steps:
(1) pretreatment is softened: carry out copper and copper alloy ingot blank softening furnace cooling after heat treatment, to blank sample analysis tissue
And crystallite dimension state；
(2) multidirectional compression cycle extrusion: first blank is compressed along blank short transverse；Then blank is overturn 90 °, edge
Charge length direction is compressed；Again blank is overturn 90 °, be compressed along blank width direction；So circulation is repeatedly；Complete
A micronization processes to blank crystallite dimension, makes blank crystallite dimension reach submicron order；
(3) roundingization processes: carries out blank shape rotating 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 processes: promote blank generation static recovery, eliminates the stress collection of blank tissue in multidirectional compression extruding
In；
(5) movable matrix reverses extruding: being placed in by blank in the die that can rotate vertically, blank is in the effect of upper mold drift
The plastic deformation that lower generation is certain, after being adjacent to concave die cavity, die rotates along extrusion axis simultaneously, promotes that blank occurs 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, makes blank crystallite dimension reach micro/nano level；
(6) microstructure sample analysis: analyze blank and soften pretreatment state, multidirectional squeezed state, low temperature destressing state, movable matrix
Reverse tissue change and the degree of grain refinement of As-extruded.
The method that Compound Extrusion prepares micro-nano copper is reversed in multidirectional compression the most as claimed in claim 1, it is characterised in that step
(2) deformation temperature of the multidirectional compression cycle extrusion described in is room temperature, Uniaxial Compression deflection 30～60%, by sampling point
Analysis guarantees that blank average grain size is less than 10 μm.
The method that Compound Extrusion prepares micro-nano copper is reversed in multidirectional compression the most as claimed in claim 1, it is characterised in that step
(5) movable matrix described in reverses extruding makes blank that three grades of necking down deformation to occur, and necking down circle diameter of bore diminishes step by step, deformation
Amount reduces step by step, and necking down deflection at different levels is not less than 30%.
The method that Compound Extrusion prepares micro-nano copper is reversed in multidirectional compression the most as claimed in claim 3, it is characterised in that described
The upper cone angle of necking down circle be 120 ± 5, lower cone angle beta is 20 ± 3.
The method that Compound Extrusion prepares micro-nano copper is reversed in multidirectional compression the most as claimed in claim 1, and described die is along squeezing
Last item rotates with 0.5rad/s ~ 5rad/s angular velocity.
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| CN201610676583.9A CN106269971B (en) | 2016-08-17 | 2016-08-17 | A kind of method that multidirectional compression torsion Compound Extrusion prepares micro-nano copper |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107081343A (en) * | 2017-06-20 | 2017-08-22 | 重庆理工大学 | A kind of continuous plastic working mould of magnesium alloy profiles and forming method |
| CN109127754A (en) * | 2018-08-29 | 2019-01-04 | 重庆大学 | A kind of preparation method of ultra-fine grained magnesium alloy extruded bars |
| CN111944958A (en) * | 2020-07-26 | 2020-11-17 | 杨军 | Preparation method of high-strength block 316L stainless steel |
| CN114134438A (en) * | 2021-11-30 | 2022-03-04 | 中国兵器工业第五九研究所 | Preparation method of fine-grain weak-texture tissue blank for shaped charge liner |
| CN115161451A (en) * | 2021-04-06 | 2022-10-11 | Oppo广东移动通信有限公司 | Rotating shaft, surface treatment equipment and surface treatment method thereof, and electronic equipment |
| CN116174588A (en) * | 2023-04-27 | 2023-05-30 | 中北大学 | Forward extrusion preparation mold for inner and outer double-layer metal bars and bar preparation method |
| CN116422718A (en) * | 2023-03-08 | 2023-07-14 | 湖州金钛导体技术有限公司 | Continuous spinning reducing processing method and manufacturing method of copper-tin-iron alloy micro-fine wire |
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| CN115161451A (en) * | 2021-04-06 | 2022-10-11 | Oppo广东移动通信有限公司 | Rotating shaft, surface treatment equipment and surface treatment method thereof, and electronic equipment |
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| CN116422718A (en) * | 2023-03-08 | 2023-07-14 | 湖州金钛导体技术有限公司 | Continuous spinning reducing processing method and manufacturing method of copper-tin-iron alloy micro-fine wire |
| CN116422718B (en) * | 2023-03-08 | 2023-11-07 | 湖州金钛导体技术有限公司 | Continuous spinning reducing processing method and manufacturing method of copper-tin-iron alloy micro-fine wire |
| CN116174588A (en) * | 2023-04-27 | 2023-05-30 | 中北大学 | Forward extrusion preparation mold for inner and outer double-layer metal bars and bar preparation method |
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