CN103343303B - A kind of Equal-channel Angular Pressing prepares the method for fine crystalline metal material - Google Patents
A kind of Equal-channel Angular Pressing prepares the method for fine crystalline metal material Download PDFInfo
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- CN103343303B CN103343303B CN201310285115.5A CN201310285115A CN103343303B CN 103343303 B CN103343303 B CN 103343303B CN 201310285115 A CN201310285115 A CN 201310285115A CN 103343303 B CN103343303 B CN 103343303B
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Abstract
The invention belongs to technical field of metal material formation, be specifically related to a kind of method that Equal-channel Angular Pressing prepares fine crystalline metal material.First metal ingot blank is squeezed into pole by the present invention on extrusion machine, then the cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity is made, on cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, blank is rotated θ clockwise or counterclockwise, 0 ° of < θ <, 90 ° or 90 ° < θ < 180 °, carry out lower a time extruding again, carry out 2 ~ 12 passages altogether, obtain the Metal with Fine Grain extruded material of grain refining.The inventive method, by expending extrusion path, improves the thinning effect of ECAP, reduces extruding passage, expands the range of application of ECAP.
Description
Technical field
The invention belongs to technical field of metal material formation, be specifically related to a kind of method that Equal-channel Angular Pressing prepares fine crystalline metal material.
Background technology
According to Hall-Petch funtcional relationship, the mean sizes of crystal grain is less, and the resistance to deformation of metal is larger; Meanwhile, grain-size reduces, and the toughness index of metal also can improve, and therefore metal microstructure refinement is the effective means simultaneously improving Strength of Metallic Materials and toughness.Equal-channel Angular Pressing (EqualChannelAngularProcessing, be called for short ECAP) be a kind of large plastometric set working method utilizing pure shear distortion to realize material grains refinement, be one of important method of the block super fine crystal material of acquisition at present, caused the very big concern of domestic and international material circle.The eighties in 20th century is Equal Channel Angular Pressing proposed by the former Russian scholar Segal, constant at the cross-sectional area carrying out sample in ECAP extrusion process, therefore, can realize successfully obtaining sub-micron crystal even nanocrystalline material to the severe plastic deformation of material by multi-pass extruding, therefore this technology not only has good researching value, also has boundless application prospect.
In Equal-channel Angular Pressing, extruding passage and metal by passage time direction very important for the refinement of microstructure.At present, per sample in the difference of every time sense of rotation and angle, the operational path of Equal-channel Angular Pressing has four kinds of paths, as shown in Figure of description Fig. 1, and path A: after every time extruding, sample non rotating, directly carries out lower a time extruding; Path B
a: after every time extruding, sample replaces rotation by 90 ° and extrudes; Path B
c: after every time extruding, sample, by same direction half-twist, enters lower a time; Path C: after every time extruding, after sample rotates 180 °, enter lower a time.According to current bibliographical information, be all that traditionally this several processing route carries out simultaneous test, research processing route, on the impact of material grains thinning effect, has but drawn the different experimental results seeming contradiction.And up to the present, take which kind of processing route can there is no unified understanding by crystal grain thinning most effectively, not yet find the most effective extrusion deformation process route, and it is most important to solve this difficult problem.
The above-mentioned classification to ECAP route has certain limitation, have ignored circular specimen can between adjacent passage the freedom of angle of rotation, square coupons can only the integral multiple of half-twist between adjacent passage, and circular specimen is quite different, it can before entering next extruding passage any rotation.And although existing ECAP method has many good qualities, but also Shortcomings part, such as production efficiency is low, usually the distortion of multi-pass will be carried out, just can obtain evenly tiny crystal grain, therefore be badly in need of finding metallic substance to carry out the optimum extruding path of ECAP distortion, reduce extruding passage, enhance productivity.
Summary of the invention
For prior art Problems existing, the invention provides a kind of method that Equal-channel Angular Pressing prepares fine crystalline metal material, object is by expending extrusion path, improves the thinning effect of ECAP, reduces extruding passage, expands the range of application of ECAP.
The technical scheme realizing the object of the invention is carried out according to following steps:
(1) first metal ingot blank is squeezed into pole on extrusion machine, then makes the cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, by blank angle of rotation θ clockwise or counterclockwise, 0 ° of < θ <, 90 ° or 90 ° < θ < 180 °, carry out lower a time extruding again, carry out 2 ~ 12 passages altogether, obtain the Metal with Fine Grain extruded material of grain refining.
Compared with prior art, feature of the present invention and beneficial effect are:
(1) lubricant is applied in mold cavity equably by the present invention before cold extrusion, extrusion stem is surperficial and extrusion is surperficial, suitable surface treatment and lubrication are carried out to extrusion, can make in Cold Extrusion Process, acquisition is suitable for Plastic Deformation Conditions, thus greatly reduce frictional coefficient, reduce load, reduce die wear, extend its work-ing life;
(2) metallic substance Grain Refinement Mechanisms is generally in extrusion process repeatedly, first, coarse grain is ground into a series of subgrain with small angle interfacial, and subgrain elongates along certain orientation and forms banded structure, and subgrain bandwidth is generally several microns or several submicron; Then, subgrain is continued to destroy, and starts the equiaxed grain structure that appearance part has wide-angle interface; Finally, subgrain band disappears, and microstructure is mainly the equiaxed grain structure with high-angle boundary;
In existing conventional extrusion process, by the integral multiple being defined as 90 ° or 90 ° in the extruding path of extrusion, and the present invention adopts circular metal sample any rotation θ between every time extruding of ECAP, dynamic → the dislocation tangling that staggers in place forms the traditional route of integral multiple dislocation wall → substructure → low angle boundary → big angle crystal boundary chain being obviously better than be only 90 ° or 90 °, this is the angle due to adjacent passage shear surface, be conducive to starting and slippage of dislocation, thus accelerate the evolution of above-mentioned chain, utilize this extruding path can greatly reduce the ECAP passage of metallic substance, boost productivity,
For the metallic substance with different crystal structure, as long as select suitable extrusion mould, and rotate suitable angle in extrusion process, make the shear plane of sample adjacent 2 extruding in ECAP process mutually to complete a business transaction into close to slip plane between the angle of angle, just greatly can improve thinning effect, shorten extruding flow process;
Particularly for the metal of plasticity difference, such as, magnesium alloy is the metal of close-packed hexagonal structure, at room temperature slip system is few, plasticity is poor, in traditional pressing method extrusion passes more after can crack, which limits the application of ECAP method in these alloys, and adopt pressing method new in the present invention, will greatly widen the application scope of ECAP technology.
Accompanying drawing explanation
Fig. 1 is the method route schematic diagram of Equal-channel Angular Pressing in prior art;
Fig. 2 comparison diagram that to be the embodiment of the present invention 1 extrude through the macrostructure of the thin brilliant high-purity aluminum material of 2 passages extruding preparations and existing method 2 passage;
Wherein: (a) is for adopting path B
cextruding; B () is 135 path extruding in embodiment 1; C () is for adopting path A extruding; D () extrudes for adopting path C;
Fig. 3 is the TEM pattern comparison diagram that the embodiment of the present invention 1 extrudes through thin brilliant high-purity aluminum material and the employing path Bc of 2 passage extruding preparations;
Wherein: (a) is 135 path extruding in embodiment 1; B () is for adopting path B
cextruding;
To be the embodiment of the present invention 2 adopt path B through the macrostructure of the thin brilliant high-purity aluminum material of 8 passages extruding preparations and prior art to Fig. 4
cthe macrostructure's comparison diagram after every time extruding of the high-purity aluminum material that 8 passage extruding obtain is carried out in extruding;
Wherein: (a) is for before extruding; B () carries out 1 passage extruding for adopting 135 paths of embodiment 2; C () carries out 2 passage extruding for adopting embodiment 2 path Bc; D () is for carrying out 2 passage extruding in employing 135 path; E () carries out 4 passage extruding for adopting path Bc; F () is for carrying out 4 passage extruding in employing 135 path; G () carries out 6 passage extruding for adopting path Bc; H () is for carrying out 6 passage extruding in employing 135 path; (i) for adopting path Bc to carry out 8 passage extruding; J () is for carrying out 8 passage extruding in employing 135 path.
Fig. 5 is the macrostructure figure of thin brilliant high-purity aluminum material prepared by the embodiment of the present invention 3;
Fig. 6 is the macrostructure figure of thin brilliant high-purity aluminum material prepared by the embodiment of the present invention 4;
Fig. 7 is the macrostructure figure of aluminium alloy grained material after 2,3 and 4 passage extruding prepared by the embodiment of the present invention 5;
Wherein: (a) is through 2 passage extruding; B () is through 3 passage extruding; C () is through 4 passage extruding;
Fig. 8 is the macrostructure figure of aluminium alloy grained material after 2,3 and 4 passage extruding adopting existing path Bc to extrude preparation;
Wherein: (a) is through 2 passage extruding; B () is through 3 passage extruding; C () is through 4 passage extruding;
Fig. 9 is the macrostructure figure of magnesium alloy grained material after 1,2,3 and 4 passage extruding prepared by the embodiment of the present invention 6;
Wherein: (a) is through 1 passage extruding; B () is through 2 passage extruding; C () is through 3 passage extruding; D () is through 4 passage extruding;
Figure 10 is that the macrostructure of magnesium alloy grained material after 1,2,3 and 4 passage extruding adopting existing path Bc to extrude preparation schemes wherein: (a) is through 1 passage extruding; B () is through 2 passage extruding; C () is through 3 passage extruding; D () is through 4 passage extruding.
Embodiment
Lubricant used in the embodiment of the present invention is MoS
2lubricant.
Carrying out observing the instrument detected to the macrostructure of gained fine crystalline metal material is SZX16 body formula mirror.
Embodiment 1
(1) the 5N5 rafifinal ingot blank of Φ 150mm × 300mm is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 135 °, carry out 2 passages altogether, obtain the thin brilliant extruded material of rafifinal of grain refining.
In order to verify beneficial effect of the present invention, selecting paths B
c, A and C carry out 2 passages extruding contrast experiments, in legacy paths, in prior art, generally believe path B
c, namely extrusion enters when lower a time extrudes best by the grain refining effect of the metallic substance prepared by the half-twist of same direction, and therefore, we observe contrast five kinds of processing route grain refining effects, as shown in Figure 2, and B
cafter route extruding, grain-size is about 200 μm, A route is about 300 μm, C route is 500 ~ 600 μm, 135 routes of the present embodiment are about 50 μm, thinning effect is the most obvious, this demonstrate that and adopt circular metal sample can any rotation between every time extruding of ECAP, reach the effect of grain refining equally, and have to be not necessarily the integral multiple of 90 ° or 90 °.
The thin brilliant high-purity aluminum material of the present embodiment and the TEM pattern comparison diagram adopting path Bc to extrude, the as can be seen from the figure situation of the rear intra-die substructure of extruding.B
cafter route extrudes 2 passages, the existence of a large amount of dislocation in structure cell, can be seen, and there occurs the entanglement of dislocation, and after 135 routes extrude 2 passages, structure cell inside almost there is no dislocation, the dislocation of crystal boundary has fully been reset and has reacted, dislocation wall is clear, and crystal boundary is tending towards straight.
Embodiment 2
(1) the 5N5 rafifinal ingot blank of Φ 150mm × 300mm is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 135 °, carry out 8 passages altogether, obtain the thin brilliant extruded material of rafifinal of grain refining.
In order to compare explanation further, under identical condition, after blank being rotated in a clockwise direction 90 °, carrying out next passage extruding, namely adopting path Bc, carrying out 8 passage extruding altogether, obtain the thin brilliant extruded material of rafifinal of grain refining.
The macrostructure of the thin brilliant high-purity aluminum material that the embodiment of the present invention 2 is prepared through 8 passage extruding and prior art adopt path B
cextruding carries out the comparison diagram of the high-purity aluminum material that 8 passage extruding obtain as shown in Figure 4, and as can be seen from Figure 4 two kinds of modes can make crystal grain obtain refinement, but B
cthe rafifinal macrostructure of route and 135 routes contrasts, and 135 routes only extrude and are just equivalent to traditional optimal route B for 2 times
cextrude the thinning effect of 8 times, the thinning effect of 135 routes the 2nd passage (Fig. 4 (d)) significantly increases in addition, and existence one suddenlys change compared with the 1st passage (Fig. 4 (b)), and this phenomenon cannot be explained with traditional refined model.
Visible, adopt circular metal sample can any rotation between every time extruding of ECAP, reach the effect of grain refining equally, and have to be not necessarily the integral multiple of 90 ° or 90 °.
Embodiment 3
(1) the 5N5 rafifinal ingot blank of Φ 150mm × 300mm is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 45 °, carry out 8 passages altogether, obtain the thin brilliant extruded material of rafifinal of grain refining, as shown in Figure 5, the aluminium grain structure as can be seen from Figure 5 adopting the pressing method of the present embodiment to obtain obtains effective refinement to its macrostructure figure.
Embodiment 4
(1) the 5N5 rafifinal ingot blank of Φ 150mm × 300mm is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 60 °, carry out 8 passages altogether, obtain the thin brilliant extruded material of rafifinal of grain refining, its macrostructure figure as shown in Figure 6, as can be seen from Figure 6 the aluminium grain structure adopting the pressing method of the present embodiment to obtain is less than 200 μm, and grain structure obtains effective refinement.
Embodiment 5
(1) 2A12 aluminum alloy holding poles is extruded into Φ 15mm pole on press, then makes the Φ 15 × 60mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould, extrude in 250 DEG C, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 135 °, carry out 4 passages altogether, obtain the thin brilliant extruded material of aluminium alloy of grain refining, its every time extruding macrostructure figure as shown in Figure 7.
In order to contrast, under similarity condition, adopt path B
ccarry out 4 passages extruding and obtain aluminium alloy thin brilliant extruded material, the macrostructure figure of its every time extruding as shown in Figure 8.
As can be seen from Figures 7 and 8, with the increase of deformation degree of extrusion, precipitate size significantly reduces, and distribution becomes even, and the thinning effect of 135 routes is better.
Embodiment 6
(1) ZK60 magnesium alloy ingot blank is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould, extrude in 250 DEG C, tongue and the tongue tail of extrusion is cut after every time extruding terminates, next passage extruding is carried out after blank being rotated in a clockwise direction 135 °, carry out 4 passages altogether, obtain the thin brilliant extruded material of aluminium alloy of grain refining, its every time extruding macrostructure figure as shown in Figure 9.
In order to contrast, under similarity condition, adopt path B
ccarry out 4 passages extruding and obtain aluminium alloy thin brilliant extruded material, the macrostructure figure of its every time extruding as shown in Figure 10.
As can be seen from Fig. 9 and Figure 10, with the increase of deformation degree of extrusion, original grain is stretched fragmentation in a certain direction, and in alloy, recrystal grain increases, and has occurred a large amount of tiny recrystal grain at grain boundaries, organize relatively uniform, homogeneous grain size improves, and the ratio shared by small grains increases gradually, and the thinning effect of 135 routes is better than path Bc.
Embodiment 7
(1) ZK60 magnesium alloy ingot blank is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould, extrude in 250 DEG C, tongue and the tongue tail of extrusion is cut after every time extruding terminates, carry out next passage extruding after blank is rotated 160 ° in the counterclockwise direction, carry out 10 passages altogether, obtain the thin brilliant extruded material of aluminium alloy of grain refining, after testing, it organizes crystal grain to obtain effective refinement.
Embodiment 8
(1) the 5N5 rafifinal ingot blank of Φ 150mm × 300mm is extruded into Φ 40mm pole on press, then makes the Φ 40 × 120mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, during every time extruding, blank rotates clockwise 80 °, carry out 12 passage extruding altogether, obtain the thin brilliant extruded material of rafifinal of grain refining, after testing, it organizes crystal grain to obtain effective refinement.
Embodiment 9
(1) 2A12 aluminum alloy holding poles is extruded into Φ 15mm pole on press, then makes the Φ 15 × 60mm cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould, extrude in 250 DEG C, tongue and the tongue tail of extrusion is cut after every time extruding terminates, carry out next passage extruding after blank is rotated 100 ° along inverse pin direction, carry out 6 passages altogether, obtain the thin brilliant extruded material of rafifinal of grain refining, after testing, it organizes crystal grain to obtain effective refinement.
Claims (1)
1. Equal-channel Angular Pressing prepares a method for fine crystalline metal material, carries out according to following steps:
(1) first metal ingot blank is squeezed into pole on extrusion machine, is then made into the cylinder blank matched with the diameter dimension of extrusion mould cylindrical cavity;
(2) at cylinder blank surface, extrusion die profile and extrusion stem surface smear lubricant, cylinder blank is placed in extrusion mould and extrudes, tongue and the tongue tail of extrusion is cut after every time extruding terminates, it is characterized in that: by blank angle of rotation θ clockwise or counterclockwise, θ=135 °, carry out lower a time extruding again, carry out 2 ~ 12 passages altogether, obtain the Metal with Fine Grain extruded material of grain refining.
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| RU2562591C1 (en) * | 2014-04-25 | 2015-09-10 | федеральное государственное автономное образовательное учреждение высшего образования "Нижегородский государственный университет им. Н.И. Лобачевского" | Method of manufacture of long-length metal bars with nanocrystal structure for medical products (versions) |
| CN105886850A (en) * | 2016-06-22 | 2016-08-24 | 广西冶金研究院有限公司 | Method for preparing aluminum-scandium master alloy with fine intermetallic compound particles |
| 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 |
| CN107282666A (en) * | 2017-06-16 | 2017-10-24 | 航天精工股份有限公司 | A kind of high intensity aluminum or aluminum alloy fastener and its manufacture method |
| CN107177806A (en) * | 2017-07-25 | 2017-09-19 | 吉林大学 | A kind of preparation method with the tough high solid solution content of magnesium aluminium alloy of superplastic height |
| CN107824625B (en) * | 2017-09-28 | 2019-07-23 | 东北大学 | A kind of room temperature high-efficiency and continuous prepares the equal channel angular Hubbing method of the pure titanium of Ultra-fine Grained |
| CN109967544A (en) * | 2019-04-16 | 2019-07-05 | 西南交通大学 | Green body for Equal-channel Angular Pressing |
| CN113414549B (en) * | 2021-06-11 | 2023-06-20 | 兰州理工大学 | Preparation method of large-size high-strength high-conductivity M2 Cu with superfine crystal structure |
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| CN101856678A (en) * | 2010-06-29 | 2010-10-13 | 中南大学 | Device capable of realizing accurate control of equal-channel angular extrusion processing route |
| CN102534447A (en) * | 2012-01-19 | 2012-07-04 | 河海大学 | Combination processing method for improving memory stability of Cu-Al series shape memory alloy |
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| CN101856678A (en) * | 2010-06-29 | 2010-10-13 | 中南大学 | Device capable of realizing accurate control of equal-channel angular extrusion processing route |
| CN102534447A (en) * | 2012-01-19 | 2012-07-04 | 河海大学 | Combination processing method for improving memory stability of Cu-Al series shape memory alloy |
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