CN101513644A - Preparation method for nano structure metal materials - Google Patents

Preparation method for nano structure metal materials Download PDF

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Publication number
CN101513644A
CN101513644A CN200910047693.9A CN200910047693A CN101513644A CN 101513644 A CN101513644 A CN 101513644A CN 200910047693 A CN200910047693 A CN 200910047693A CN 101513644 A CN101513644 A CN 101513644A
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China
Prior art keywords
metal material
preparation
rolling
roll
nanostructured
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CN200910047693.9A
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Chinese (zh)
Inventor
李东
徐宏
朱登亮
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East China University of Science and Technology
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East China University of Science and Technology
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Priority to CN200910047693.9A priority Critical patent/CN101513644A/en
Publication of CN101513644A publication Critical patent/CN101513644A/en
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Abstract

The invention relates to a preparation method for nano structure metal materials with nano structure characteristics. In particular, the invention relates to a method for preparing metal with nano structure characteristics based on plastic distortion principle. In the temperature range of 4-1600k, the generating plastic distortion is repeatedly and regularly rolled by high speed revolution and rolling in the controllable treating ambience condition so that the macro crystal microscopic structure of the metal materials to be treated is thinned to the nano structure. The preparation method is particularly suitable for industrial mass production of the large-scale nano structure metal materials.

Description

A kind of preparation method of nano structure metal materials
Technical field
The present invention relates to have the preparation method of the metal material of nanostructured feature, specifically, the present invention relates to a kind of metal material that preparation has the nanostructured feature based on theory of plastic deformation.
Background technology
Nano structure metal materials is meant that microstructure (at least on a yardstick) has the single-phase or heterogeneous metal (comprising simple metal and alloy) of nanofeature.Because nano metal material has high defect concentration with respect to traditional metal materials, as the room, dislocation, sub boundary, crystal boundary etc., nano material has usually and is different from, and is better than the excellent properties of corresponding coarse grain material usually, as the mechanical property of excellence, high diffusion, good electricity, magnetic performance etc.
Up to now, developed the multiple preparation method who relates to nano structure metal materials.Can be divided into by its different preparation were established: (a) preparation method from bottom to top, as ball milling hot pressing, vapor condensation, electro-deposition etc.; (b) top-down preparation method, as equal channel angle extruding, stacked rolling closed etc.But above-mentioned preparation method is because there are some shortcomings in intrinsic limitation itself, and inevitably there is hole in the nano structure metal materials prepared as the ball milling pressure sintering, contaminating impurity and problem such as not fine and close; The equal channel angle pressing method only can prepare circle or square-section sample, and prepared material shape is subjected to very big restriction, and needs the large-tonnage press device; The stacked method of closing of rolling exists hole and rolling interlayer in conjunction with problem.When there is various microscopic defect in above preparation technology's prepared nano material, also be difficult to prepare the large scale material, to satisfy the engineering actual demand, especially as the demand of structural material aspect.Therefore preparation of nanomaterials be always the restriction nano materials research carry out in a deep going way and engineering on the main bottleneck of extensive use.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano structure metal materials, it is simple that this preparation method has technology, prepared nano metal material size is big, be easy to characteristics such as large-scale industrial production, and easily dock, have wide industrial basis and using value with the preparation technology of traditional metal materials.Adopt the nano structure metal materials of the present invention's preparation to have advantages such as pollution-free, complete densification.Proposition of the present invention will make nano structure metal materials become possibility as the widespread adoption of function and structural material.
Technical scheme of the present invention is:
The invention provides the preparation method of a kind of macro nanometer structural metal, the employed device of this preparation method is the described device of the applicant in the application for a patent for invention of submitting on the same day " a kind of method and device thereof for preparing nano structure superficial layer of metal materials ", is made up of piece-holder and motion, roll, roll motion, temperature atmosphere controlling organization, transmission mechanism and driving mechanism etc.Utilization makes it that plastic deformation take place around the repeatedly rolling described metal material of roll that the revolution axis rotates at a high speed, by introducing the purpose that the high density crystal defect reaches refinement microstructure.Described roll rotates freely around the rotation axis when rolling, and described metal material and described roll are done relative motion clocklike by set track simultaneously.Usually, motion mode has two kinds: motion mode one, and described roll only rotates, and the Plane of rotation holding position is constant, promptly roll does not have translational motion, and processed described metal material is done translational motion by set track with the speed of coupling; Motion mode two, motionless, the described roll of processed described metal material is done translational motion with the speed of coupling by set track in revolution, and the movement locus of described roll covers pending described metal material fully.
In the rolling, can pass through heater; as electrical heating; or cooling medium; as liquid helium, liquid hydrogen, liquid nitrogen, dry ice etc.; pending metal material is heated or cools off to regulate the temperature of described pending metal material; or feed inert gas, nitrogen, hydrogen etc. and protect, or feed carburizing, nitriding atmosphere reactive to satisfy the demand of different nanostructured metals preparations, obtain simple substance or composite nanostructure metal to realize different treatment process.
Wherein, the roll revolution speed can be adjusted between 0.1~20000rpm to obtain different strain rates, satisfies the requirement that different metal material is handled.Roller diameter can be adjusted between 1~2000mm to satisfy the demand of different application occasion to nanostructured metal.
The movement locus and the speed of pending metal material do not have specific (special) requirements, but the surface that should guarantee pending metal material is covered fully, be that pending metal material surface is rolled down to fully, and guarantee the registration of rolling vestige more than 5%, and registration choose with the rolling degree of depth closely related.
Generally speaking, the present invention can realize the preparation of complete nano structure metal materials by three kinds of different process routes.Process route one, after described metal material simultaneously is rolled out the nanostructured that certain thickness meets the demands, the upset workpiece is rolling by identical technological parameter still to be the another side relative with it of open grain structure, so that pending metallic plate all is refined as nanostructured at the tissue of thickness direction; Process route two after described metal material simultaneously is rolled out the certain thickness nanostructured that meets the demands, can adopt machinery or other to remove the material method, and removing is the material of coarse-grain structure still, obtains the metal material of complete nanostructured; Process route three, the rolling preparation nanostructured simultaneously on the metal material two sides, as adopting two but be not limited to the device of two roll, a plurality of rolls are rolling preparation nanostructured on the metal material plane of symmetry simultaneously.
The present invention has following advantage:
1, the preparation method is simple.This method is in conjunction with the advantage of traditional rolling mill practice and impact plastic strain fining metal material microstructure, and preparation technology is simple, and various technological parameters are easy to control.
2, prepared nano structure metal materials yardstick is big, is suitable for suitability for industrialized production.
3, prepared nano structure metal materials is fine and close, pollution-free fully.
4, applied widely.Theoretically, have certain plasticity, plastic deformation can take place, and can prepare nano structure metal materials by method of the present invention by the metal of plastic deformation thinning microstructure.
Description of drawings
Fig. 1 is the front view of device that method of the present invention adopts;
Fig. 2 is the left view of device that method of the present invention adopts;
Fig. 3 is the generalized section of the roll of device that method of the present invention adopts, wherein (a) and (b), (c) respectively representative profile be rectangle, symmetrical polygon and the oval-shaped roll of being with triangle.
Symbol description:
1 piece-holder and motion; 2 workpiece; 3 rotation axis; 4 rolls; 5 roll motions; 6 temperature atmosphere control device; 7 transmission mechanisms; 8 driving mechanisms; 9 revolution axis.
The specific embodiment
Below, the invention will be further described by embodiment, and it will help to understand the present invention, but not limit content of the present invention.
As Fig. 1, shown in 2, the employed device of preparation method of the present invention is by piece-holder and motion 1, roll 4, roll motion 5, temperature atmosphere controlling organization 6, transmission mechanism 7, driving mechanism 8 compositions such as grade.Concrete preparation process is: roll 4 is done revolution motion around revolution axis 9 under the drive of roll motion 5, and pending metal material clamping is done feed motion with certain speed edge perpendicular to the direction of roll plane of movement on piece-holder and motion 1.By the atmospheric condition in the temperature atmosphere controlling organization 6 adjusting preparation process and the temperature of pending metal material.Generally speaking, can realize the preparation of complete nano structure metal materials by three kinds of different process routes.Process route one, described pending metal material is simultaneously prepared after the nanostructured that meets the demands, the pending metal that overturns is rolling by identical technological parameter still to be the another side of open grain structure, all is refined as nanostructured so that pending plate thickness direction is organized.Process route two, described pending metal material is simultaneously prepared after the nanostructured that meets the demands, and can adopt machinery or other to remove the material method, and removing still is the material part of coarse-grain structure, obtains the metal material of complete nanostructured.Process route three is in rolling preparation nanostructured of metal both sides while.As adopting but be not limited to the device of two rotary rollers, two rolls can be simultaneously in the rolling preparation nanostructured of metal both sides.The profile of roll as shown in Figure 3, wherein (a) and (b) (hexagon), (c) represent the pressure roller with difformity section respectively, the stress surface of corresponding different situations on metal material; L and D are respectively the diameter and the length of roll, and its diameter is that 1~2000mm, length are 1~1000mm.
Embodiment 1
Utilize the present invention to prepare the nanostructured pure copper material.
Equipment: the applicant is in the device described in the application for a patent for invention of submitting on the same day;
Roll rotational speed: 500rpm;
Dimension of roller: 50mm;
Deformation temperature: 77k;
Rolling number of times: 60 times;
Rolling mode: the first rolling one side system another side that rerolls;
Pure copper material: purity>99.9%, 973K annealing 2 hours, crystallite dimension is: 50~300 μ m.Thickness of slab 3mm.
The nanostructured pure copper material that obtains after the processing.Crystallite dimension is 90~260nm.Thickness of slab~1.5mm.
Embodiment 2
Utilize the present invention to prepare the nanostructured carbon steel material.
Equipment: the applicant is in the device described in the application for a patent for invention of submitting on the same day;
Roll rotational speed: 400rpm;
Dimension of roller: 50mm;
Deformation temperature: room temperature;
Rolling number of times: 40 times;
Rolling mode: the first rolling one side system another side that rerolls;
Carbon steel material: phosphorus content is 3.5% carbon steel, and crystallite dimension is: 50~200 μ m.Thickness of slab 2mm.
Handle the resulting nanostructured carbon steel in back.Crystallite dimension is: 30~120nm.Thickness of slab~1.0mm.

Claims (8)

1, a kind of preparation method of nano structure metal materials, it is characterized in that, the rolling described metal material of roll that utilization is rotated at a high speed around the revolution axis, described roll rotates freely around the rotation axis simultaneously when rolling, and described metal material and described roll are done relative motion clocklike by set track, repeatedly prepare the metal material with nanostructured after shearing, the compressive plastic deformation effect continuously in the operation of rolling;
The revolution speed of described roll is that 0.1~20000rpm, revolution radius are that 1~2000mm, diameter are that 1~2000mm, length are 1~1000mm; The temperature of described metal material is 4~1600K when rolling;
Described revolution axis is the horizontal middle spindle of described transmission mechanism;
Described rotation axis is the installation axis of described roll self.
2, preparation method according to claim 1, it is characterized in that described relative motion is meant: described roll is made revolution motion, and its revolution holding position, plane is constant, be that roll does not have translational motion, and processed described metal material is done translational motion by specific track with the speed of coupling; Perhaps, processed motionless, the described roll of described metal material is done translational motion with the speed of coupling by specific track in revolution.
3, preparation method according to claim 1 is characterized in that, the described operation of rolling has three kinds of process routes:
A, pending described metal material are simultaneously prepared after the nanostructured that meets the demands, the pending metal material that overturns, by the rolling and prepared nanostructured that goes out of identical technological parameter relative still be the another side of open grain structure;
B, pending described metal material are partly prepared after the nanostructured that meets the demands, and removing still is the part material of coarse-grain structure, the metal material that obtains having nanostructured;
C, on the two sides of pending described metal material symmetry rolling preparation nanostructured simultaneously.
4, according to the arbitrary described preparation method of claim 1~3, it is characterized in that, adjust the temperature of pending described metal material in the described operation of rolling by heating or cooling medium; Simultaneously, adopt protective atmosphere or atmosphere reactive, prepare the described nano structure metal materials of simple substance or composite construction.
According to the arbitrary described preparation method of claim 1~3, it is characterized in that 5, the movement velocity of described metal material is 0.1~20000mm/min when rolling.
6, preparation method according to claim 4 is characterized in that, the mode of described heating is electrical heating, and described cooling medium is one or more in liquid helium, liquid hydrogen, liquid nitrogen and the dry ice.
7, preparation method according to claim 4 is characterized in that, described protective atmosphere is inert gas, nitrogen or hydrogen; Described atmosphere reactive is carburizing atmosphere or nitriding atmosphere.
8, according to the arbitrary described preparation method of claim 1~3, it is characterized in that, described roll has 2,4 or 6 of symmetry, is rolled operation at the plane of symmetry simultaneously, synchronous or asynchronously at the rolling preparation nano structure metal materials of the plane of symmetry of described metal material.
CN200910047693.9A 2009-03-17 2009-03-17 Preparation method for nano structure metal materials Pending CN101513644A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102051461A (en) * 2011-01-25 2011-05-11 大冶市亚光高强螺栓有限公司 Surface strengthening method for magnetic yoke pull rod
CN102059250A (en) * 2010-11-09 2011-05-18 燕山大学 Electro-plastic two-roll mill of low-temperature liquid nitrogen cooling medium
CN104948653A (en) * 2015-04-27 2015-09-30 陈曦 Production method of buffering and energy-absorbing nano fluid
CN106040955A (en) * 2016-08-24 2016-10-26 江苏金源高端装备股份有限公司 Forging process of gear shaft
CN107881310A (en) * 2017-12-23 2018-04-06 陕西理工大学 The method that carbon steel surface prepares non crystalline structure layer
CN109943696A (en) * 2017-12-21 2019-06-28 中国科学院金属研究所 A method of precipitation strengthening alloy intensity is improved using matrix nano structure

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102059250A (en) * 2010-11-09 2011-05-18 燕山大学 Electro-plastic two-roll mill of low-temperature liquid nitrogen cooling medium
CN102051461A (en) * 2011-01-25 2011-05-11 大冶市亚光高强螺栓有限公司 Surface strengthening method for magnetic yoke pull rod
CN102051461B (en) * 2011-01-25 2013-03-06 大冶市亚光高强螺栓有限公司 Surface strengthening method for magnetic yoke pull rod
CN104948653A (en) * 2015-04-27 2015-09-30 陈曦 Production method of buffering and energy-absorbing nano fluid
CN106040955A (en) * 2016-08-24 2016-10-26 江苏金源高端装备股份有限公司 Forging process of gear shaft
CN109943696A (en) * 2017-12-21 2019-06-28 中国科学院金属研究所 A method of precipitation strengthening alloy intensity is improved using matrix nano structure
CN107881310A (en) * 2017-12-23 2018-04-06 陕西理工大学 The method that carbon steel surface prepares non crystalline structure layer

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Open date: 20090826