CN102925832A - Large plastic deformation method for preparing superfine twin crystal copper - Google Patents

Large plastic deformation method for preparing superfine twin crystal copper Download PDF

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CN102925832A
CN102925832A CN2012104268532A CN201210426853A CN102925832A CN 102925832 A CN102925832 A CN 102925832A CN 2012104268532 A CN2012104268532 A CN 2012104268532A CN 201210426853 A CN201210426853 A CN 201210426853A CN 102925832 A CN102925832 A CN 102925832A
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annealing
rolling
copper
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王军丽
刘润
周蕾
史庆南
黄启祥
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Kunming University of Science and Technology
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Abstract

The invention provides a large plastic deformation method for preparing superfine twin crystal copper. The method comprises the step of asymmetrical accumulative rolling-bonding and a subsequent heat treatment annealing process, raw material preparation, homogenizing annealing, surface polishing, the asymmetrical accumulative rolling-bonding, deformation and annealing are conducted to obtain a superfine twin crystal copper material. According to the method, a large deformation asymmetrical accumulative rolling-bonding technology is supplemented with annealing heat treatment, by the aid of the shear stress and a cumulative strain effect during an asymmetrical accumulative rolling-bonding process, the stacking staggered arrangement and grain refinement inside a material are promoted, the forming of the twin crystal is promoted through a annealing heat treatment process, and a novel continuous preparation method is provided for the further study on a metal material strengthening technology. According to the method, the size and the shape of the material are not changed before and after processing, the restriction of total strain in a thickness direction of a conventional rolling sheet material is overcome, the deformation capacity is increased, the quality of the surface of the product is improved, the production efficiency is high, the process is simple, a large-size metal sheet material can be produced, and the industrial production is easy to achieve.

Description

A kind of large plastometric set method for preparing ultra-fine twin copper
Technical field
The invention belongs to the Plastic working " technical field, be specifically related to the method that the asynchronous ply rolling of a kind of gross distortion prepares ultra-fine twin material.
Background technology
Super fine crystal material has unique small grains and high-density Grain Boundary Character, shows the performance of a series of excellences such as high strength and good toughness, wear resistance, makes super fine crystal material become the focus of domestic and international research.Twin boundary is a kind of low energy coherent grain boundary, in that it can hinder dislocation motion effectively in the plastic history as conventional crystal boundary, have with conventional Grain-Boundary Phase like strengthening effect, simultaneously its slip plane of can be used as again dislocation absorbs a large amount of dislocations and is conducive to viscous deformation.It is a kind of new way of material reinforcement that the twin reinforcement now is known as in the world, by introducing a large amount of twin boundaries can increase substantially the intensity of material its electroconductibility is had no significant effect.Ultra-fine/nano twin crystal copper becomes important source material in the industrial sectors such as aviation, machinery, electrical instrumentation, chemical industry owing to having small special thin Jingjing circle structure, application prospect is extremely wide, and it also will produce important promotion to association areas such as superconducting magnet technology, electrical power transmission system, dynamoelectric equipment and MEMS (micro electro mechanical system), also will produce material impact to the development of Ultra-fine Grained/nanocrystalline material technology.
Find that by the relevant literature published at home and abroad the method for preparing at present Ultra-fine Grained/nano twin crystal copper mainly contains pulse electrodeposition method, plastic deformation method, magnetron sputtering method etc.For example Chinese Academy of Sciences's metal Lu Ke (referring to Lu L, Chen X, Huang X, Qian L, Lu K. Ultrahigh strength and high electrical conductivity in copper[J] .Science, 2004 (304): 422-426.) adopt the pulse electrodeposition method to prepare highdensity nano twin crystal copper, its tensile yield strength can reach 900MPa, breaking tenacity is up to 1068MPa (being about more than 10 times of common fine copper), and has and the suitable room-temperature conductivity of (97%IACS) of oxygen-free high-conductivity copper; Lu Qiuhong is (referring to Lu Qiuhong, Zhao Weisong, Sui Manling. the research [J] of the nano twin crystal steel structure of dynamic plastic deformation preparation under the liquid nitrogen temperature. Acta Metallurgica Sinica, 2006,42 (9): 909-913.) adopt the dynamic plasticity distortion to send out and successfully prepared nano twin crystal copper; M.D.Merz(is referring to Merz M D, Dahlgren S D. Tensile strength and work hardening of ultrafine-grained high-purity copper[J]. Journal of Applied Physics, 1976,46 (8): 3235-3237.) adopt magnetron sputtering method to prepare nano twin crystal copper, find that twin boundary can effectively hinder dislocation motion.But these methods all difficult large-scale industrialization that realizes are produced Ultra-fine Grained/nanocrystalline twin copper.
As far back as 1998, Japanese scholars Saito Y has proposed to adopt the accumulation sandwich rolling process to prepare the large plastic forming technology of agglomerate body thin plate ultrafine grain metal material, the method is applied to copper and copper alloy, aluminium alloy, IF steel and stratified composite etc. by success, is widely used in the production of aerospace, automobile stratified material.Asynchronous ply rolling method a kind of super fine crystal material preparation method who reduces rolling pressure, improves the strip working (machining) efficiency that to be the nineties in 20th century grow up on accumulation ply rolling technology and Differential speed rolling technology basis.Compare with the accumulation sandwich rolling process, asynchronous ply rolling method owing to exist to rub with the hands in the distorted area roll be out of shape and strong promotion the refinement of material compound and crystal grain of material interface in plastic history.Through further retrieval, not yet find to utilize asynchronous ply rolling technology to prepare ultra-fine twin material.
Summary of the invention
The present invention proposes a kind of sever Plastic Deformation for preparing ultra-fine twin copper-asynchronous ply rolling method (Asymmetrical Accumulative Rolling Bonding, AARB) first.
The present invention realizes by following technical proposal: a kind of sever Plastic Deformation for preparing ultra-fine twin copper comprises asynchronous ply rolling step and subsequent heat-treatment of annealing technique, the process following process steps:
(1) raw-material preparation: the length and width needs according to reality cut the copper coin material, and thickness is got 0.5~2.5mm;
(2) homogenizing annealing: 350~600 ℃ of lower insulation annealings 1~2.5 hour, furnace cooling carried out homogenizing annealing again with step (1) gained starting material, to obtain uniform tissue and to reduce the residualinternal stress of material internal;
(3) surface finish: because the material surface oxidation is serious behind the homogenizing annealing, can affect the compound of interface, be polished in the surface of material behind step (2) homogenizing annealing, then blow with remaining copper powder and the impurity of hair dryer with the surface;
(4) asynchronous ply rolling distortion: two alignment of material after step (3) polishing are stacking, then obliquity is fixed and polished to a wherein end along its length, be convenient to milling train nip, carry out again asymmetrical rolling; Subsequently the sheet material after rolling is cut off section's raw edges and burr carry out surface finish again, and be then that two block of material are stacking, carries out asymmetrical rolling again, so repeats 6~10 passages; During this time, in the asymmetrical rolling process, after every ply rolling two passages, be that 100~150 ℃ of lower insulation 30~60min carry out stress relief annealing once in annealing temperature, mainly be in order to reduce macroscopical internal stress of fine copper; This step is under the prerequisite that keeps copper strip, rely on shear-stress in the asynchronous ply rolling process and accumulation strain effect to promote the compound of the refinement of the wrong row of stacking, crystal grain of material internal and interface, for the formation of heat-treatment of annealing process twin tissue provides a large amount of potential motives;
(5) annealing: the sheet material after the asynchronous ply rolling of step (4) is placed in the heat treatment furnace, under 100~250 ℃ of conditions, be incubated 5~120min, to eliminate the unrelieved stress of the course of processing, in answer or recrystallization annealing process, carry out crystal boundary optimization, slippage by the annealing process Dislocations and climbing makes the change of local dot matrix and crystal boundary planar orientation, promotes the formation of twin in the annealing process, then cool to room temperature with the furnace and take out, namely obtain ultra-fine twin copper material.
The polishing of described step (3) is to polish along length direction with wire wheel brush, observe while polishing, until wildness is coarse, reflective evenly till.
The obliquity of described step (4) is 25~35 °.
The asynchronous ratio of the asymmetrical rolling of described step (4) is 1.08~1.15, draft is 50%.
The inventive method has following clear superiority: the present invention adopts the asynchronous ply rolling technology of gross distortion to be aided with annealing thermal treatment, rely on shear-stress and the wrong row of stacking of accumulation strain effect promotion material internal and the refinement of crystal grain in the asynchronous ply rolling process, promote again the formation of twin by annealing heat treatment process, for the further investigation of the intensifying technology of metallic substance provides a kind of new continuous production method.The present invention has kept shape and the size of material before and after processing not to change, overcome the restriction that pair rolling prepares overall strain on the sheet metal thickness direction, increased deflection, improved the quality of product surface, has high productivity, technique is simple, can produce large-sized sheet metal, is easy to realize suitability for industrialized production.
(1) the asynchronous ply rolling technology of gross distortion has high productivity, can produce large-sized sheet metal, realizes easily suitability for industrialized production;
(2) gross distortion asynchronous ply rolling technology has overcome the restriction that pair rolling prepares overall strain on the sheet metal thickness direction, has reduced rolling load, has increased deflection, has improved the quality of product surface;
(3) technique is simple, and cost is low, reduces energy consumption, and is pollution-free, realized can obtaining uniform ultra-fine twin copper after the asynchronous ply rolling of less passage is aided with annealing thermal treatment.
Description of drawings
Fig. 1 is pure copper samples optical texture pattern behind embodiment 1 homogenizing annealing;
Fig. 2 is the micro-organization chart of embodiment 1 pure copper samples rolling surface after the asynchronous ply rolling of 6 passages;
Fig. 3 is embodiment 1 pure copper samples vertical section optical texture figure after the asynchronous ply rolling of 6 passages;
Fig. 4 is that embodiment 1 is through the transmission electron microscope micro-organization chart of pure copper samples after the asynchronous ply rolling of 6 passages behind annealing 45min under 190 ℃ of conditions.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) raw-material preparation: cut T2 fine copper sheet material, length is got 300mm, the wide 25mm of getting, thickness is got 1mm; The content of this T2 fine copper sheet material sees the following form 1:
Table 1
Figure 219261DEST_PATH_IMAGE001
(2) homogenizing annealing: with step (1) gained starting material in KS-4000 type intelligent temperature control box heat treatment furnace with 600 ℃ of lower insulation annealings 1 hour, furnace cooling carries out homogenizing annealing again, to obtain to organize and reduce uniformly the residualinternal stress of material internal; Material structure is more even behind the homogenizing annealing, and grain-size is at 20~40 μ m, as shown in Figure 1;
(3) surface finish: because the material surface oxidation is serious behind the homogenizing annealing, can affect the compound of interface, with the surface of material behind step (2) homogenizing annealing with wire wheel brush with rotating speed 300 turn/min polishes along length direction, observe while polishing, until wildness is coarse, reflective evenly till, then blow with remaining copper powder and the impurity of hair dryer with the surface;
(4) asynchronous ply rolling distortion: two alignment of material after step (3) polishing are stacking, then 30 ° obliquity is fixed and polished to a wherein end along its length, be convenient to milling train and nip, carry out asymmetrical rolling again, its asynchronous ratio is 1.08, draft is 50%; Subsequently the sheet material after rolling is cut off section's raw edges and burr carry out surface finish again, and be then that two block of material are stacking, carries out asymmetrical rolling again, so repeats 6 passages; During this time, in the asymmetrical rolling process, after every ply rolling two passages, be that 130 ℃ of lower insulation 30min carry out stress relief annealing once in annealing temperature, mainly be in order to reduce macroscopical internal stress of fine copper; This step is under the prerequisite that keeps copper strip, rely on shear-stress in the asynchronous ply rolling process and accumulation strain effect to promote the compound of the refinement of the wrong row of stacking, crystal grain of material internal and interface, for the formation of heat-treatment of annealing process twin tissue provides a large amount of potential motives; The Geometrical change of material is as shown in table 2, and material is by obviously refinement after the asynchronous ply rolling of six passages, and average grain size is 1 μ m, as shown in Figure 2; The compound phase of vertical section is a good, and not observed does not have obvious interface, as shown in Figure 3;
Figure 998998DEST_PATH_IMAGE002
(5) annealing: the sheet material after the asynchronous ply rolling of step (4) is placed in the KS-4000 type intelligent temperature control box heat treatment furnace, under 190 ℃ of conditions, be incubated 45min, to eliminate the unrelieved stress of the course of processing, in answer or recrystallization annealing process, carry out crystal boundary optimization, slippage by the annealing process Dislocations and climbing makes the change of local dot matrix and crystal boundary planar orientation, promotes the formation of twin in the annealing process, then cool to room temperature with the furnace and take out, namely obtain ultra-fine twin copper material.
The result shows:
Asynchronous ply rolling technology is because two different linear resonance surface velocities of work roll surface, change the direction of metal friction power, in the distorted area of material, exist to rub with the hands and roll the distorted area, strongly promoted the compound of the refinement of crystal grain and material interface, obtained the Ultra-fine grain copper that average crystal grain is about 1 μ m after the asynchronous ply rolling of six passages, as shown in Figure 3; Do not observed obvious interface this moment, as shown in Figure 4; Having obtained average crystal grain behind 190 ℃ of annealing 45 min is 2 μ m, and the twin lamellae mean thickness is the ultra-fine twin copper of 1.5 μ m.Asynchronous ply rolling process has increased shear-stress, promoted the wrong row of stacking of copper material inside, and the wrong row of stacking can be increased in generation twin nucleus quantity in answer or the recrystallization annealing process, accumulation strain has reached the effect of crystal grain thinning simultaneously, the size of the front crystal grain of answer or recrystallization annealing and the size of the rear twin of annealing have been controlled, in the slippage of annealing process Dislocations with climb, make the change of local dot matrix and crystal boundary planar orientation, promoted the formation of twin in the annealing process.This shows that asynchronous ply rolling is aided with effectively crystal grain thinning of annealing heat treatment technology, promote the formation of twin, obtain ultra-fine twin copper, have good application prospect.
Embodiment 2
(1) raw-material preparation: the length and width needs according to reality cut the copper coin material, and thickness is got 0.5mm;
(2) homogenizing annealing: 400 ℃ of lower insulation annealings 1.5 hours, furnace cooling carried out homogenizing annealing again with step (1) gained starting material, to obtain uniform tissue and to reduce the residualinternal stress of material internal;
(3) surface finish: because the material surface oxidation is serious behind the homogenizing annealing, can affect the compound of interface, polished along length direction with wire wheel brush in the surface of material behind step (2) homogenizing annealing, observe while polishing, until wildness is coarse, reflective evenly till, then blow with remaining copper powder and the impurity of hair dryer with the surface;
(4) asynchronous ply rolling distortion: two alignment of material after step (3) polishing are stacking, then 25 ° obliquity is fixed and polished to a wherein end along its length, be convenient to milling train and nip, carry out asymmetrical rolling again, its asynchronous ratio is 1.15, draft is 50%; Subsequently the sheet material after rolling is cut off section's raw edges and burr carry out surface finish again, and be then that two block of material are stacking, carries out asymmetrical rolling again, so repeats 8 passages; During this time, in the asymmetrical rolling process, after every ply rolling two passages, be that 150 ℃ of lower insulation 40min carry out stress relief annealing once in annealing temperature, mainly be in order to reduce macroscopical internal stress of fine copper; This step is under the prerequisite that keeps copper strip, rely on shear-stress in the asynchronous ply rolling process and accumulation strain effect to promote the compound of the refinement of the wrong row of stacking, crystal grain of material internal and interface, for the formation of heat-treatment of annealing process twin tissue provides a large amount of potential motives;
(5) annealing: the sheet material after the asynchronous ply rolling of step (4) is placed in the heat treatment furnace, under 250 ℃ of conditions, be incubated 5min, to eliminate the unrelieved stress of the course of processing, in answer or recrystallization annealing process, carry out crystal boundary optimization, slippage by the annealing process Dislocations and climbing makes the change of local dot matrix and crystal boundary planar orientation, promotes the formation of twin in the annealing process, then cool to room temperature with the furnace and take out, namely obtain ultra-fine twin copper material.
Embodiment 3
(1) raw-material preparation: cut the copper coin material, length is got 200mm, the wide 50mm of getting, thickness is got 2.5mm;
(2) homogenizing annealing: 350 ℃ of lower insulation annealings 2.5 hours, furnace cooling carried out homogenizing annealing again with step (1) gained starting material, to obtain uniform tissue and to reduce the residualinternal stress of material internal;
(3) surface finish: because the material surface oxidation is serious behind the homogenizing annealing, can affect the compound of interface, polished along length direction with wire wheel brush in the surface of material behind step (2) homogenizing annealing, observe while polishing, until wildness is coarse, reflective evenly till, then blow with remaining copper powder and the impurity of hair dryer with the surface;
(4) asynchronous ply rolling distortion: two alignment of material after step (3) polishing are stacking, then 35 ° obliquity is fixed and polished to a wherein end along its length, be convenient to milling train and nip, carry out asymmetrical rolling again, its asynchronous ratio is 1.12, draft is 50%; Subsequently the sheet material after rolling is cut off section's raw edges and burr carry out surface finish again, and be then that two block of material are stacking, carries out asymmetrical rolling again, so repeats 10 passages; During this time, in the asymmetrical rolling process, after every ply rolling two passages, be that 100 ℃ of lower insulation 60min carry out stress relief annealing once in annealing temperature, mainly be in order to reduce macroscopical internal stress of fine copper; This step is under the prerequisite that keeps copper strip, rely on shear-stress in the asynchronous ply rolling process and accumulation strain effect to promote the compound of the refinement of the wrong row of stacking, crystal grain of material internal and interface, for the formation of heat-treatment of annealing process twin tissue provides a large amount of potential motives;
(5) annealing: the sheet material after the asynchronous ply rolling of step (4) is placed in the heat treatment furnace, under 100 ℃ of conditions, be incubated 120min, to eliminate the unrelieved stress of the course of processing, in answer or recrystallization annealing process, carry out crystal boundary optimization, slippage by the annealing process Dislocations and climbing makes the change of local dot matrix and crystal boundary planar orientation, promotes the formation of twin in the annealing process, then cool to room temperature with the furnace and take out, namely obtain ultra-fine twin copper material.
The above example has only been expressed embodiments of the present invention and experimental result, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that under the prerequisite that does not break away from patent design of the present invention can also make some distortion and improvement, these all belong to the protection domain of patent of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (4)

1. sever Plastic Deformation for preparing ultra-fine twin copper is characterized in that: comprise asynchronous ply rolling step and subsequent heat-treatment of annealing technique, through following process steps:
(1) raw-material preparation: the length and width needs according to reality cut the copper coin material, and thickness is got 0.5~2.5mm;
(2) homogenizing annealing: 350~600 ℃ of lower insulation annealings 1~2.5 hour, furnace cooling carried out homogenizing annealing again with step (1) gained starting material;
(3) surface finish: polished in the surface of material behind step (2) homogenizing annealing, then remaining copper powder and the impurity with the surface blows;
(4) asynchronous ply rolling distortion: two alignment of material after step (3) polishing are stacking, then obliquity is fixed and polished to a wherein end along its length, carry out again asymmetrical rolling; Subsequently the sheet material after rolling is cut off section's raw edges and burr carry out surface finish again, and be then that two block of material are stacking, carries out asymmetrical rolling again, so repeats 6~10 passages; During this time, in the asymmetrical rolling process, after every ply rolling two passages, be that 100~150 ℃ of lower insulation 30~60min carry out stress relief annealing once in annealing temperature;
(5) annealing: the sheet material after the asynchronous ply rolling of step (4) is incubated 5~120min under 100~250 ℃ of conditions, then cools to room temperature with the furnace and take out, namely obtain ultra-fine twin copper material.
2. the sever Plastic Deformation of the ultra-fine twin copper of preparation according to claim 1, it is characterized in that: the polishing of described step (3) is to polish along length direction, observe while polishing, until wildness is coarse, reflective evenly till.
3. the sever Plastic Deformation of the ultra-fine twin copper of preparation according to claim 1 and 2, it is characterized in that: the obliquity of described step (4) is 25~35 °.
4. the sever Plastic Deformation of the ultra-fine twin copper of preparation according to claim 1 and 2 is characterized in that: the asynchronous ratio of the asymmetrical rolling of described step (4) is 1.08~1.15, draft is 50%.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104651765A (en) * 2013-11-21 2015-05-27 青岛润鑫伟业科贸有限公司 Copper sheet made through severe plastic deformation technology
CN104894497A (en) * 2015-06-04 2015-09-09 合肥美的电冰箱有限公司 Preparation method of nano-twin cooper piece, nano-twin copper piece, evaporator and refrigerator
CN105772504A (en) * 2015-12-27 2016-07-20 佛山市领卓科技有限公司 Method for improving strength and plasticity of pure metal
CN106637001A (en) * 2016-12-20 2017-05-10 中南大学 Continuous asymmetrical rolling preparation method for gradient strip
CN109647882A (en) * 2018-08-14 2019-04-19 南京交通职业技术学院 A kind of high-strength high-plastic nano-stack material and preparation method thereof
CN111570513A (en) * 2020-05-25 2020-08-25 江苏联峰实业有限公司 Fine-grain gear steel and preparation method thereof
CN114686789A (en) * 2022-04-12 2022-07-01 福建工程学院 Method for improving pure copper grain boundary corrosion resistance by increasing proportion of coherent twin grain boundary

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
周蕾等: "异步累计叠轧纯铜再结晶温度、时间对孪晶的影响", 《热加工工艺》 *
王军丽等: "大变形异步叠轧技术制备高强高导超细晶铜材研究", 《航空材料学报》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104651765A (en) * 2013-11-21 2015-05-27 青岛润鑫伟业科贸有限公司 Copper sheet made through severe plastic deformation technology
CN104894497A (en) * 2015-06-04 2015-09-09 合肥美的电冰箱有限公司 Preparation method of nano-twin cooper piece, nano-twin copper piece, evaporator and refrigerator
CN105772504A (en) * 2015-12-27 2016-07-20 佛山市领卓科技有限公司 Method for improving strength and plasticity of pure metal
CN106637001A (en) * 2016-12-20 2017-05-10 中南大学 Continuous asymmetrical rolling preparation method for gradient strip
CN106637001B (en) * 2016-12-20 2018-11-06 中南大学 A kind of continuous asymmetrical rolling preparation method in the surface layer of gradient band
CN109647882A (en) * 2018-08-14 2019-04-19 南京交通职业技术学院 A kind of high-strength high-plastic nano-stack material and preparation method thereof
CN111570513A (en) * 2020-05-25 2020-08-25 江苏联峰实业有限公司 Fine-grain gear steel and preparation method thereof
CN114686789A (en) * 2022-04-12 2022-07-01 福建工程学院 Method for improving pure copper grain boundary corrosion resistance by increasing proportion of coherent twin grain boundary
CN114686789B (en) * 2022-04-12 2023-09-01 福建工程学院 Method for improving pure copper grain boundary corrosion resistance by increasing coherent twin boundary proportion

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Application publication date: 20130213