CN105779723B - A kind of metal material and preparation method thereof having both intensity and plasticity - Google Patents
A kind of metal material and preparation method thereof having both intensity and plasticity Download PDFInfo
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- CN105779723B CN105779723B CN201510987542.7A CN201510987542A CN105779723B CN 105779723 B CN105779723 B CN 105779723B CN 201510987542 A CN201510987542 A CN 201510987542A CN 105779723 B CN105779723 B CN 105779723B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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Abstract
The present invention provides a kind of metal material and preparation method thereof for having both intensity and plasticity.The material is characterized in that: the crystal grain in its microscopic structure is made of the crystal grain of two kinds of different grain size ranges of thickness, and coarse grain forms ribbon and is distributed in fine grain.Coarse grain is that conventional micron is brilliant, and fine grain is nanocrystalline；Nanocrystalline particle size range is 10-200 nanometers, and the particle size range of micron crystalline substance is 0.5 micron -10 microns.Preparation method by preparing multilayer material, cold rolling, recrystallization form.
Description
Technical field
The present invention relates to a kind of preparation method of metal material, especially a kind of intensity and all excellent metal of plastic property
Material and preparation method thereof.
Background technique
Sheet metal is generally obtained using the method for forging or rolling at present, can be divided into high temperature according to the difference of temperature and be added
Work and room temperature are processed.As mechanical structure part, intensity (commonly using tensile strength, yield strength etc. to characterize) is (common to prolong with plasticity
Stretch rate, contraction percentage of area etc. to characterize) be metal material two most important mechanical properties.High intensity can be such that metal is occurring
Big load is undertaken before plastic deformation, and big plasticity can then make it carry out biggish plastic deformation before destruction, avoid
Unexpected brittle fracture occurs.As engineering material, it is generally desirable to high-intensitive materials still to obtain high-strength material by people
While, the plasticity of general meeting loss material；Improve plasticity while, then can loss material intensity.The two is conflict,
It can not generally get both.
Chinese patent 1887513 provides a kind of high-efficient production technology of high pure aluminium foil for electrolytic capacitor.Mainly include
The cross-shear rolling step and heat treatment step of high-purity aluminum foil, the method have the characteristics that, use speed ratio for 1.05~1.30
Differential speed rolling technology, controls the rolling deformation state and rolling texture configuration of aluminium foil, i.e. the rolling Jing Guo less passage obtains big
The high-purity aluminum foil of deformation quantity.The continuous annealing in protective atmosphere, final production go out the high-purity aluminum foil containing extremely strong cubic texture.With this
High pure aluminium foil for electrolytic capacitor made from the method for invention has the advantage that 1. asymmetrical rolling Product Precisions compare pair rolling
Improve level-one；2. { 100 } face cubic texture occupancy rate is up to 95% or more.
Chinese patent 101569892 proposes a kind of AZ31 magnesium alloy asynchronous longitudinal and transverse tandem rolling method, it is characterised in that,
It is demarcated including treating rolled alloy, first time rolling then is carried out to alloy using two roller asynchronous rolling machines, will be rolled for the first time
Alloy after system carries out second of rolling again.It is 10 Μ M that resulting AZ31 alloy grain average-size, which will be rolled, by the invention,
Mechanical property after optimization rolling can achieve elongation percentage 16.73%, yield strength 249.2MPA, tensile strength 319.46MPA.
105080966 A of Chinese patent CN provides a kind of preparation method of nanocrystalline metal strip in razor-thin, according to the following steps
Carry 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, the different speed-ratio regulation step-length, pre-pressing force of asynchronous very thin hoop mill are set
With front and back tensile stress；(3) starting milling train carries out a passes to rolled piece, on-line control friction speed ratio when rolling (；4) measurement is rolled
The thickness of part, and mill speed, friction speed ratio, different speed-ratio regulation step-length, front and back tension and pre-pressing force are set again；
(5) starting milling train carries out next passes to rolled piece, on-line control friction speed ratio when rolling；(6) step 2 to 5 is repeated, until rolling
Part is rolling to a thickness of 1~5 μm.Method of the invention can realize the serialization of nanocrystalline metal strip in razor-thin production, and need not
Intermediate annealing.
Chinese patent 10162923 proposes a kind of preparation method of superfine crystalline pure iron, includes: selection prepared material to be rolled,
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 temperature, is made super
Fine grain pure iron.The present invention using the above scheme, by easy steps be made crystal particle scale be 0.9 Μ M, high-angle boundary (Θ >=
15 °) content reach 65% or more ultrafine-grained (UFG) microstructure.Show through uniaxial tensile test, material is surrendered by force after asymmetrical rolling
Degree is obviously improved.
Summary of the invention:
Goal of the invention: the mechanical property in order to give full play to pure metal, the present invention provide a kind of intensity and plasticity of having both
The preparation method of metal material.
Technical scheme is as follows:
Firstly, using the modes such as electrolysis, plating, deposition, gradient be cooling, by controlling preparation condition, such as change temperature, dense
The parameters such as degree prepare the structure of microstructure layering.This is because the crystallization condition of metal changes when changing parameter,
Its grain size can also change.For example, cooling using gradient, then the big region crystal grain of cooling rate is tiny, cooling in casting
Slow-footed region crystal grain is more coarse.Therefore, by changing preparation condition, can regulate and control each micro- in the sheet metal of preparation
The grain size in region is seen, to obtain the plate of grain size layering.Then using the method for asymmetrical rolling at room temperature, system
A kind of standby pure metal material for having both intensity and plasticity.When asymmetrical rolling, since its top and bottom rolls velocity of rotation is different, have
Slow roll and quick roll, contacted with slow roll material part deformation it is smaller, the change of grain size is relatively small, and with it is quick
The some materials deformation of roller contact is big, and crystal grain can become more tiny.Generally speaking, according to the present invention it is possible to prepare one kind not
Uniform microscopic structure.Crystal grain in its microscopic structure is made of the crystal grain of two kinds of different grain size ranges, a kind of for the micro- of routine
Meter Jing, one kind are nanocrystalline；Nanocrystalline particle size range is 10-200 nanometers, and the particle size range of micron crystalline substance is 0.5 micron -10
Micron.60% or more nanocrystalline volume fraction, the volume fraction of micron crystalline substance 40% hereinafter, micron crystalline substance be embedded in it is nanocrystalline
In, form belt structure.
Specific preparation method the following steps are included:
1. selecting pure metal material: control Oxygen in Metals content is less than 0.1%；All impurity elements are less than 0.5%；
2. such as changing temperature, concentration by controlling preparation condition using modes such as electrolysis, plating, deposition, gradient coolings
Etc. parameters, it is every use one group of parameter, prepare layer of material, then use another group of parameter, prepare another layer material, so
Repeatedly, the multi-layered board under different preparation conditions can be prepared.From the point of view of microscopic structure, which shows layered structure,
One face crystal grain of plate is relatively tiny, is set as the face A, and another side crystal grain is more coarse, is set as the face B；
3. starting Multi-functional rolling system, the speed ratio of top and bottom rolls, speed ratio 1.1-1.5 are set；Setting rolls shape every time
Variable is 1-8%；The speed of low speed roller is set as 0.5-2 meter per second；
3. starting main driving motor, start the operation of rolling；
4. after once rolling, repetition (2) (3) process 15 times or more；
5. carrying out full annealed heat treatment.Recrystallization temperature is the one third of the melting point metal to a quarter, when
Between 3-20 minutes.
Beneficial effect: using pure metal material prepared by the present invention, can have both micron brilliant outstanding plasticity and nanometer
Brilliant excellent intensity.In fact, being not only difficult to prepare, and plasticity is very poor by the nanocrystalline metal material constituted entirely.And this hair
The material of bright preparation, not only simple more in preparation method, plasticity is high.And also it is better than in intensity nanocrystalline.Its root
Source is that this material structure can achieve greatly back processing hardening, this is not present in the material of even grained.Together
When, Bauschinger effect enhances the intensity of material.For Direct Rolling, it is aobvious that the present invention has made multilayer before rolling
Micro texture further enhances the differentiation distribution of material internal crystal grain.In addition, the present invention uses room temperature rolling, than working as
Before the high temperature rolling that generallys use it is more energy saving, it is at low cost, be suitable for large-scale production.
Detailed description of the invention
Fig. 1 is micro-organization chart of the invention, biggish brilliant for micron, be distributed in it is tiny it is nanocrystalline in.
Specific embodiment
Below by conjunction with attached drawing and embodiment detailed description of the present invention preparation method, but do not constitute to limit of the invention
System.
Embodiment 1
1. configuring copper-bath: the concentration of copper is 60g/l, and the concentration of sulfuric acid concentration 40g/l, Cl are 20ppm, temperature
It is 40 degrees Celsius, current density 50A/dm2, when the thickness of layers of copper reaches 50 microns, layers of copper 1 is obtained, then changes parameter
Are as follows: the concentration of sulfuric acid concentration 120g/l, Cl are 60ppm, and temperature is 65 degrees Celsius, current density 60A/dm2.Obtain layers of copper
2,61 microns of thickness；Electrolytic parameter 1 is used again, obtains layers of copper 3,65 microns of thickness；Finally using point solution parameter 1, layers of copper is obtained
4,68 microns of thickness；
2. starting Multi-functional rolling system, the speed ratio of top and bottom rolls, speed ratio 1.1 are set；Set each rolling deformation amount
It is 6%；The speed of low speed roller is set as 2 meter per seconds；
3. starting main driving motor, start the operation of rolling, wherein layers of copper 1 is contacted with slow roll；
4. repeating rolling 15 times after once rolling；
5. carrying out full annealed heat treatment, recrystallization temperature is 300 degrees Celsius, the time 8 minutes.
Fabric analysis: the average grain size of micron crystalline substance is 3.1 microns, and nanocrystalline average grain diameter is 110 nanometers.
Embodiment 2
1. configuring copper-bath: the concentration of copper is 100g/l, and the concentration of sulfuric acid concentration 60g/l, Cl are 50ppm, temperature
Degree is 40 degrees Celsius, current density 50A/dm2, when copper layer thickness reaches 120 microns, layers of copper 1 is obtained, then changes parameter
Are as follows: the concentration of sulfuric acid concentration 130g/l, Cl are 80ppm, and temperature is 65 degrees Celsius, current density 80A/dm2.Obtain layers of copper
2,132 microns of thickness.Electrolytic parameter 1 is used again, obtains layers of copper 3,130 microns of thickness；
2. starting Multi-functional rolling system, the speed ratio of top and bottom rolls, speed ratio 1.2 are set；Set each rolling deformation amount
It is 2%；The speed of low speed roller is set as 1 meter per second；
3. starting main driving motor, start the operation of rolling, wherein layers of copper 1 is contacted with slow roll；
4. repeating rolling 12 times after once rolling；
5. carrying out full annealed heat treatment, recrystallization temperature is 270 degrees Celsius, the time 3 minutes.
Fabric analysis: the average grain size of micron crystalline substance is 9.5 microns, and nanocrystalline average grain diameter is 65 nanometers.
Embodiment 3
1. selecting pure titanium target material, oxygen content 0.08%；
2. being deposited in magnetic control sputtering system: being evacuated to 10-3Pa is filled with argon gas, is then evacuated to 10 again- 3Pa, adjustment operating voltage are 400V, sputter duty ratio 70%, start to carry out sputtering sedimentation titanium plate；When the thickness of titanium plate reaches 20
When micron, voltage is transferred to 300V, duty ratio is transferred to 40%；When the overall thickness of titanium plate reaches 40 microns, voltage is recalled to
400V, duty ratio adjust back to 70%；10 times repeatedly, the titanium plate of one piece of 10 sputtering sedimentation is obtained, system is then shut off, takes
Titanium plate out.
4. starting Multi-functional rolling system, the speed ratio of top and bottom rolls, speed ratio 1.1 are set；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. repeating (2) (3) process 20 times after once rolling；
5. in 470 degrees Celsius of progress full annealed heat treatments, the time 3 minutes.
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.
Using tensile test at room temperature, the properties of product of the embodiment of the present invention are as follows: with conventionally fabricated comparison
Comparative example is conventionally fabricated metal typical performance, is micron crystal structure.It can be seen that the intensity of material of the present invention
It is the 2 times or more of micron crystalline substance, while plasticity also increases；And for nanocrystalline, the plasticity of material of the invention is big
It is better than pure nanocrystalline material greatly.
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 are also answered
It is considered as protection scope of the present invention.
Claims (4)
1. a kind of metal material for having both intensity and plasticity, it is characterised in that: crystal grain in its microscopic structure by two kinds of thickness not
The crystal grain of one-size range forms, and coarse grain forms ribbon and is distributed in fine grain；Coarse grain is that conventional micron is brilliant, carefully
Crystal grain is nanocrystalline；Nanocrystalline particle size range is 10-200 nanometers, and the particle size range of micron crystalline substance is 0.5 micron -10 microns；
Preparation method includes the following steps:
1) select metal material: oxygen content is less than 0.1%；All impurity elements are less than 0.5%；
2) every to use one group of parameter by controlling preparation condition in such a way that deposition or gradient are cooling, prepare layer of material
Later, another group of parameter is then used, another layer material is prepared, repeatedly, can prepare under different preparation conditions
Multi-layered board；From the point of view of microscopic structure, which shows layered structure, and a face crystal grain of plate is relatively tiny, is set as the face A,
Another side crystal grain is more coarse, is set as the face B；
3) start Multi-functional rolling system, set the speed ratio of top and bottom rolls, speed ratio 1.1-1.5；Set each rolling deformation
Amount is 1-8%；The speed of low speed roller is set as 0.5-2 meter per second；
4) start main driving motor, start the operation of rolling；
5) it after to once roll, repeats 3) 4) process 15 time or more；
6) full annealed heat treatment is carried out.
2. a kind of metal material for having both intensity and plasticity as described in claim 1, it is characterised in that: nanocrystalline volume point
60% or more number, the volume fraction of micron crystalline substance is below 40%.
3. a kind of preparation method for the metal material for having both intensity and plasticity as described in claim 1 again, it is characterised in that: tie
Brilliant temperature is the one third of the melting point metal to a quarter, time 3-20 minute.
4. a kind of preparation method for the metal material for having both intensity and plasticity as described in claim 1, it is characterised in that: rolling
Temperature is room temperature.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353720A (en) * | 2007-07-23 | 2009-01-28 | 宝山钢铁股份有限公司 | Manufacturing method of metallic plate having superfine crystal continuous gradient tissue and metallic plate |
| CN102009504A (en) * | 2010-02-10 | 2011-04-13 | 湘潭大学 | Steel strip plated with multi-layer micron/nano-crystal nickel films and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100595292C (en) * | 2007-06-15 | 2010-03-24 | 中国科学院金属研究所 | High speed processing method for realizing superfine crystal grain structure on metallic material surface |
| CN101348869B (en) * | 2007-07-16 | 2010-06-02 | 南京理工大学 | Preparation of crystal grain size controllable bimodal distribution block superfine/nanocrystalline alloy |
| CN102161051A (en) * | 2010-10-29 | 2011-08-24 | 东北大学 | Asynchronous rolling method for forming nano structure on surface of metal sheet |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353720A (en) * | 2007-07-23 | 2009-01-28 | 宝山钢铁股份有限公司 | Manufacturing method of metallic plate having superfine crystal continuous gradient tissue and metallic plate |
| CN102009504A (en) * | 2010-02-10 | 2011-04-13 | 湘潭大学 | Steel strip plated with multi-layer micron/nano-crystal nickel films and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Heterogeneous lamella structure unites ultrafine-grain strength with coarse-grain ductility;Xiaolei Wu等;《Proceed of the National Academy of Science of the United States of America》;20151124;第112卷(第47期);14501-14505 |
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