CN105772504B - The method for improving simple metal intensity and plasticity - Google Patents
The method for improving simple metal intensity and plasticity Download PDFInfo
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- CN105772504B CN105772504B CN201510988166.3A CN201510988166A CN105772504B CN 105772504 B CN105772504 B CN 105772504B CN 201510988166 A CN201510988166 A CN 201510988166A CN 105772504 B CN105772504 B CN 105772504B
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 239000002184 metal Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000005096 rolling process Methods 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000001953 recrystallisation Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000001755 magnetron sputter deposition Methods 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 23
- 239000010936 titanium Substances 0.000 description 22
- 229910052719 titanium Inorganic materials 0.000 description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 20
- 229910052802 copper Inorganic materials 0.000 description 20
- 239000010949 copper Substances 0.000 description 20
- 238000004544 sputter deposition Methods 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000004062 sedimentation Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 208000018875 hypoxemia Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000006263 metalation reaction Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009718 spray deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Metal Rolling (AREA)
Abstract
The present invention provides a kind of method for improving simple metal intensity and plasticity, it is characterised in that：Using the method for magnetron sputtering and asymmetrical rolling, the method repeatedly rolled using Light deformation, room temperature is rolled into less than the 0.5~2% of original depth.The crystal grain in microscopic structure after rolling is made of the crystal grain of two kinds of different grain size ranges, and one kind is coarse grain, and one kind is fine grain；The particle size range of fine grain is 10 200 nanometers, and coarse grained particle size range is 0.3 micron -5 microns.This method is while metal strength is improved, moreover it is possible to improve the plasticity of metal.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance simple metal material, especially a kind of high-strength high-plasticity simple metal
And preparation method thereof.
Background technology
Simple metal has excellent performance, but in general intensity is not high, therefore usually uses the means system of alloying
It is standby to promote its intensity into alloy, but this loss plasticity.For the processing method of simple metal, it is typically limited to high temperature pressure
Processing.The intensity and plasticity of simple metal can be improved simultaneously, be the target that research worker pursues.
105080966 A of Chinese patent CN provide a kind of preparation method of nanocrystalline metal strip in razor-thin, according to the following steps
It carries out:(1) raw material used for steel, copper, aluminium, nickel, titanium or molybdenum ribbon material, or above-mentioned metal alloy strip steel rolled stock as rolled piece, thickness
It is 200~5000 μm；(2) mill speed, friction speed ratio, different speed-ratio regulation step-length, the pre-pressing force of asynchronous very thin hoop mill are set
With front and rear tensile stress；(3) start milling train and one passes is carried out to rolled piece, on-line control friction speed ratio during rolling (；4) it measures and rolls
The thickness of part, and mill speed, friction speed ratio, different speed-ratio regulation step-length, front and rear tension and pre-pressing force are set again；
(5) start milling train and carry out next passes to rolled piece, on-line control friction speed ratio during rolling；(6) step 2 to 5 is repeated, until rolling
It is 1~5 μm that part, which is rolling to thickness,.The method of the present invention can realize the serialization of nanocrystalline metal strip in razor-thin production, and need not
Intermediate annealing.
104846363 A of Chinese patent CN propose a kind of preparation method of nanostructured Titanium board, a kind of nanostructured
The preparation method of Titanium board, including such as next stage:(1) selection of titanium valve particle:High purity titanium powder of hypoxemia, low hydrogen is selected,
The particle size distribution range of titanium valve particle is 5-200 μm；(2) high speed spray deposition prepares Titanium board base:Titanium valve particle is accelerated,
High speed titanium valve particle is collided with substrate, makes titanium valve particle that strong plastic deformation occur and deposit to form Titanium board base；(3) slab
Heat treatment:Obtained Titanium board base is heat-treated；(4) hot rolling.Metallic titanium plate crystallite dimension prepared by this method is tiny,
To be nanocrystalline, even tissue is had excellent performance, and overcomes the shortcomings that Titanium board intensity is low, hardness for 2 times of common Titanium board with
On, while the advantages that inherit the excellent corrosion resisting property of common Titanium board, heat resistance and biocompatibility.Present invention process letter
List, controllability is good, production efficiency is high, contributes to industrial applications.
Chinese patent 10162923 proposes a kind of preparation method of superfine crystalline pure iron, including:Prepared material to be rolled is selected,
5 hours are kept the temperature at 900 DEG C；Symmetric rolling and the rolling of asynchronous friction speed；Second synchronization rolling is carried out after heat preservation at normal temperatures, is made super
Fine grain pure iron.Crystal particle scale is made as 0.9 Μ M using the above scheme, by easy steps in the present invention, high-angle boundary (Θ >=
15 °) content reach more than 65% ultrafine-grained (UFG) microstructure.Show through uniaxial tensile test, material is surrendered by force after asymmetrical rolling
Degree is obviously improved.
Invention content：
Goal of the invention：In order to excavate the potential of simple metal material, simple metal intensity is improved simultaneously the present invention provides a kind of
With the method for plasticity.The ductility of simple metal can only be usually extended within 10000% by conventional calendering processing, for some
The material processed is difficult to, such as magnesium alloy and titanium alloy, ductility is then very low.And the present invention uses micro-machined method,
It is rolled under room temperature, the ductility of the simple metal of the cubic systems such as copper can be extended to more than 50000%, the metals such as magnesium, titanium
Ductility can also reach more than 5000%.Crystal grain in the microscopic structure of simple metal after processing is by two kinds of different grain size ranges
Crystal grain forms, and one kind is coarse grain, and one kind is fine grain；The particle size range of fine grain is 10-200 nanometers, coarse grained granularity
Range is 0.3 micron -5 microns.Wherein more than 70% volume fraction of Jingjing grain, coarse grained volume fraction 30% hereinafter,
Coarse grain is distributed in fine grain.The intensity of the simple metal is high, and excellent plasticity.
Technical scheme is as follows:
Using simple metal as target, the simple metal plank of microscopic structure layering is prepared.Asymmetrical rolling is used at room temperature
Method, each deformation amount controlling is within 5%, using multiple rolling, the thickness of final simple metal original thickness 0.5~
Thus 2% hereinafter, prepare a kind of simple metal material of high intensity.
Specific preparation method includes the following steps：
1. the simple metal plank of microscopic structure layering is prepared as target using simple metal；
2. starting Multi-functional rolling system, the fast ratio of top and bottom rolls is set, speed is than being 1.1-1.3；Setting rolls shape every time
Variable is 1-5%；The speed of low speed roller is set as 0.5-2 meter per seconds；
3. starting main driving motor, start the operation of rolling；
4. treating after once rolling, repeat to roll, until thickness is thinned to less than the 0.5~2% of original thickness；
5. carrying out full annealed heat treatment, recrystallization temperature arrives a quarter for 1/3rd of the simple metal fusing point,
Time 3-20 minute；
Beneficial effect：Processing method using the present invention can fully excavate the ductility of simple metal, and ductility is most
Height can reach more than 100000%, more than any report data in available data.The present invention can obtain high ductility and prepare
Simple metal, existing coarse grain in institutional framework, and have fine grain can have both the outstanding plasticity of coarse grain and fine grain is excellent
Different intensity.In fact, the metal material being made of entirely fine grain, is not only difficult to prepare, and plasticity is very poor.And present invention system
Standby material, not only intensity is high, but also plasticity is high, is even better than fine grain in intensity.It has its source in this material knot
Structure can reach greatly back of the body processing hardening, generate apparent Bauschinger effect.In addition, the present invention is compared using room temperature rolling
It is energy saving, it is at low cost, suitable for large-scale production.
Description of the drawings
Fig. 1 is the micro-organization chart of the present invention, larger for coarse grain, tiny for fine grain.
Specific embodiment
Below by with reference to attached drawing and embodiment detailed description of the present invention preparation method, but the limit to the present invention is not formed
System.
Embodiment 1
1. fine copper is selected to be deposited in magnetic control sputtering system as target：It is evacuated to 10-3Pa is filled with argon gas, so
It is evacuated to 10 again afterwards-3Pa, adjustment operating voltage are 600V, sputter duty ratio 70%, proceed by sputtering sedimentation copper coin；Work as copper
When the thickness of plate reaches 150 microns, voltage is transferred to 300V, duty ratio is transferred to 40%；When the overall thickness of copper coin reaches 300 microns
When, voltage is recalled into 600V, duty ratio adjusts back to 70%；It is so repeated, until copper plate thickness reaches 18 millimeters, takes out copper
Plate；
2. starting Multi-functional rolling system, the fast ratio of top and bottom rolls is set, speed is than being 1.2；Set each rolling deformation amount
It is 3%；The speed of low speed roller is set as 0.5 meter per second；
3. starting main driving motor, start the operation of rolling；
4. treating after once rolling, repeat to roll, until thickness is thinned to 15 microns；
5. carrying out full annealed heat treatment, recrystallization temperature is 250 degrees Celsius, 20 minutes time.
Fabric analysis：Coarse grained average grain size is 1.5 microns, and the average grain diameter of fine grain is 90 nanometers.
Embodiment 2
1. the pure titanium target material of selection, is deposited in magnetic control sputtering system：It is evacuated to 10-3Pa is filled with argon gas, Ran Houzai
It is evacuated to 10-3Pa, adjustment operating voltage are 400V, sputter duty ratio 70%, proceed by sputtering sedimentation titanium plate；When titanium plate
When thickness reaches 20 microns, voltage is transferred to 300V, duty ratio is transferred to 40%；It, will when the overall thickness of titanium plate reaches 40 microns
Voltage recalls to 400V, and duty ratio adjusts back to 70%；So 10 times repeatedly, obtain the titanium plate of one piece of 10 sputtering sedimentation, Ran Houguan
System is closed, takes out titanium plate；
2. starting Multi-functional rolling system, the fast ratio of top and bottom rolls is set, speed is than being 1.1；Set each rolling deformation amount
It is 2%；The speed of low speed roller is set as 0.5 meter per second；
3. starting main driving motor, start to roll；
4. treating after once rolling, (2) (3) process is repeated 20 times；
5. carry out full annealed heat treatment, 3 minutes time at 470 degrees Celsius.
The results show that the average grain size of micron crystalline substance is 2.4 microns, nanocrystalline average grain diameter is for metallographic microanalysis
89 nanometers.
Embodiment 3
1. fine copper is selected to be deposited in magnetic control sputtering system as target：It is evacuated to 10-3Pa is filled with argon gas, so
It is evacuated to 10 again afterwards-3Pa, adjustment operating voltage are 600V, sputter duty ratio 70%, proceed by sputtering sedimentation copper coin；Work as copper
When the thickness of plate reaches 100 microns, voltage is transferred to 300V, duty ratio is transferred to 40%；When the overall thickness of copper coin reaches 200 microns
When, voltage is recalled into 600V, duty ratio adjusts back to 70%；It is so repeated, until copper plate thickness reaches 1 millimeter, takes out copper
Plate；
2. starting Multi-functional rolling system, the fast ratio of top and bottom rolls is set, speed is than being 1.2；Set each rolling deformation amount
It is 3%；The speed of low speed roller is set as 0.8 meter per second；
3. starting main driving motor, start the operation of rolling；
4. treating after once rolling, repeat to roll, until thickness is thinned to 0.8 micron；
5. carrying out full annealed heat treatment, recrystallization temperature is 280 degrees Celsius, 3 minutes time.
Fabric analysis：Coarse grained average grain size is 0.35 micron, and the average grain diameter of fine grain is 56 nanometers.
Embodiment 4
1. fine copper is selected to be deposited in magnetic control sputtering system as target：It is evacuated to 10-3Pa is filled with argon gas, so
It is evacuated to 10 again afterwards-3Pa, adjustment operating voltage are 600V, sputter duty ratio 70%, proceed by sputtering sedimentation copper coin；Work as copper
When the thickness of plate reaches 50 microns, voltage is transferred to 300V, duty ratio is transferred to 40%；When the overall thickness of copper coin reaches 100 microns
When, voltage is recalled into 600V, duty ratio adjusts back to 70%；It is so repeated, until copper plate thickness reaches 0.5 millimeter, takes out
Copper coin；
2. starting Multi-functional rolling system, the fast ratio of top and bottom rolls is set, speed is than being 1.3；Set each rolling deformation amount
It is 1%；The speed of low speed roller is set as 2 meter per seconds；
3. starting main driving motor, start the operation of rolling；
4. treating after once rolling, repeat to roll, until thickness is thinned to 0.5 micron；
5. carrying out full annealed heat treatment, recrystallization temperature is 300 degrees Celsius, 3 minutes time.
Fabric analysis：Coarse grained average grain size is 0.24 micron, and the average grain diameter of fine grain is 24 nanometers.
Performance test：Simple metal tension test is carried out using universal testing machine, the results are shown in Table 1.As can be seen that this
The simple metal of invention maintains excellent plasticity while intensity is increased substantially.
The above is only some examples of embodiment of the present invention, it should be pointed out that：For the technology people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (4)
- A kind of 1. method for improving simple metal intensity and plasticity, it is characterised in that：Microscopic structure is prepared using magnetically controlled sputter method For the material of layering, then using the method for Light deformation, the multiple asymmetrical rolling of room temperature, be rolled into original depth 0.5~ 2% hereinafter, the crystal grain in microscopic structure after rolling is made of the crystal grain of two kinds of different grain size ranges, and one kind is a kind of for coarse grain For fine grain；The particle size range of fine grain is 10-200 nanometers, and coarse grained particle size range is 0.3 micron -5 microns, and coarse-grain The stripped distribution of grain.
- A kind of 2. method as described in claim 1 for improving simple metal intensity and plasticity, it is characterised in that：Preparation method packet Include following steps：1）Simple metal is selected to prepare the simple metal plank of microscopic structure layering as target；2）Start Multi-functional rolling system, set the fast ratio of top and bottom rolls, speed is than being 1.1-1.3;Set each rolling deformation It measures as 1-5%；The speed of low speed roller is set as 0.5-2 meter per seconds；3）Start main driving motor, start the operation of rolling；4）It treats after once rolling, repeats to roll, until the thickness of final simple metal becomes less than the 2% of original depth； 5）Carry out full annealed heat treatment.
- A kind of 3. method as claimed in claim 2 for improving simple metal intensity and plasticity, it is characterised in that：Recrystallization temperature is / 3rd of the melting point metal arrive a quarter, time 3-20 minute.
- 4. a kind of simple metal prepared by method as described in claim 1, it is characterised in that：More than 70% volume fraction of fine grain, Coarse grained volume fraction is 30% hereinafter, coarse grain is distributed in fine grain.
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| CN104846363A (en) * | 2014-02-14 | 2015-08-19 | 宝山钢铁股份有限公司 | Nanostructured pure titanium plate preparation method |
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| JP4242801B2 (en) * | 2004-03-26 | 2009-03-25 | 住友金属鉱山伸銅株式会社 | Rolled copper foil and method for producing the same |
| CN101629231A (en) * | 2009-08-20 | 2010-01-20 | 上海交通大学 | Superfine crystalline pure iron preparation method |
| CN102161051A (en) * | 2010-10-29 | 2011-08-24 | 东北大学 | Asynchronous rolling method for forming nano structure on surface of metal sheet |
| CN102321896A (en) * | 2011-09-09 | 2012-01-18 | 北京工业大学 | Nanocrystalline nickel with high-density twin structure and preparation method thereof |
| CN102925832A (en) * | 2012-10-31 | 2013-02-13 | 昆明理工大学 | Large plastic deformation method for preparing superfine twin crystal copper |
| CN103114185A (en) * | 2013-03-11 | 2013-05-22 | 上海理工大学 | Steel with multi-scale twin-crystal structure and preparation method of steel |
| CN105080966B (en) * | 2015-08-19 | 2017-04-12 | 东北大学 | Method for manufacturing ultra-thin nanocrystalline metal strip |
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| CN104846363A (en) * | 2014-02-14 | 2015-08-19 | 宝山钢铁股份有限公司 | Nanostructured pure titanium plate preparation method |
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| Title |
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| Heterogeneous lamella structure unites ultrafine-grain strength with coarse-grain ductility;Xiaolei Wu etc.;《Proceed of the National Academy of Science of the United States of America》;20151124;第112卷(第47期);第14501-14505页 * |
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