CN107841790A - A kind of preparation method for being orientated controllable Cu Al Mn shape memory alloy monocrystallines - Google Patents
A kind of preparation method for being orientated controllable Cu Al Mn shape memory alloy monocrystallines Download PDFInfo
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- CN107841790A CN107841790A CN201710981910.6A CN201710981910A CN107841790A CN 107841790 A CN107841790 A CN 107841790A CN 201710981910 A CN201710981910 A CN 201710981910A CN 107841790 A CN107841790 A CN 107841790A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/05—Alloys based on copper with manganese as the next major constituent
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
The present invention relates to a kind of preparation method for being orientated controllable Cu Al Mn shape memory alloy monocrystallines, belong to field of metal preparation.The preparation method is prepared along solidification direction using directional freeze method first to be had<001>The columnar-shaped polycrystalline Cu Al Mn blank of shape memory alloy of fiber texture degree.Then, using cycle heat treatment method, make alloy grain that continuous abnormal occur and grow up, until growing up to monocrystalline；Meanwhile by controlling cycle heat treatment system and technological parameter, ensure that crystal grain orientation does not occur substantially to change in single crystal growth process, has closely so as to obtain along initial solidification direction<001>The Cu Al Mn shape memory alloy monocrystallines of orientation.Method for preparing single crystal of the present invention realizes the tropism control in solid-state phase political reform single crystal growth process, has the advantages that large size single crystal body (monocrystalline size is up to more than 50mm) can be prepared, orientation is easily-controllable, technique is simple.
Description
Technical field
The invention belongs to field of metal preparation, is related to a kind of controllable Cu-Al-Mn shape memory alloy monocrystallines of orientation
Preparation method.
Background technology
Marmem be it is a kind of integrate perceive and the intellectual material that drives, can be made sensor, detector,
Damping device, energy converter and intelligent micro device etc., are widely used in electronic communication, health care, machine-building, boat
The various fields such as empty space flight, derived energy chemical and daily life.Cu-Al-Mn marmems are because its is cheap, shape
Memory performance is good, damping, energy absorption performance it is excellent and easy to process, it has also become most the marmem of application potential it
One, especially suitable for manufacture building, large-scale precision instrument damping device.
The super-elasticity and SME of Cu-Al-Mn marmems have significant crystallite dimension sensitiveness.With
The increase of crystallite dimension, the superelastic strain and SME of alloy significantly improve.For example, diameter 10mm's is isometric more
Crystalline substance tissue bar, when average grain size is 10 μm, its super-elasticity only has 2% or so；When average grain size increases to 10mm
When, super-elasticity can reach more than 7%；And can be more than 10% for single crystal alloy, its super-elasticity.
Traditional method for preparing single crystal such as czochralski method, Bridgeman methods etc., preparation technology is complicated, and control difficulty is big, it is difficult to
Prepare large size single crystal body.Research finds that when being heat-treated for 500 DEG C~600 DEG C, α phases separate out Cu-Al-Mn marmems,
And with forming subgrain on β phase matrixes.When alloy is heated to about more than 730 DEG C, back dissolving, subgrain tissue occur for α precipitated phases
Remain on β phase matrixes.Residual subgrain is grown up for β phase crystal grain in subsequent high temperature heat treatment process provides driving force, makes alloy β phases
Abnormal growth [Omori T., et al. (2013) .Science 341 (6153) occurs for crystal grain:1500-1502.].It may be noted that
, precipitation and the back dissolving of α phases can constantly be repeated by multiple cycle heat treatment process.Based on above-mentioned mechanism, people is studied
Member develops Cu-Al-Mn shape memory alloy monocrystallines novel preparation method [Kusama T., the et al. based on solid-state phase changes principle
(2017)Nature Communications 8(354):1-9], i.e., by polycrystalline Cu-Al-Mn blank of shape memory alloy
Implement rational cycle heat treatment, promote alloy grain abnormal growth constantly to carry out, until forming monocrystalline.This method breaches biography
System clotting method prepares the bottleneck of large size single crystal, prepared Cu-Al-Mn shape memory alloy monocrystallines size up to 10mm with
On.
But the Cu-Al-Mn marmems circle heat treatment developed at present can not be orientated to crystal grain and carry out
Control, i.e., because the common polycrystalline alloy using crystal grain random orientation is as raw material, during single crystal preparation, occur abnormal long
Big crystal grain has randomness, therefore the single-crystal orientation obtained is also random.And for Cu-Al-Mn marmems
For, the key performance such as its super-elasticity, SME has significant orientation dependence, i.e., is orientated when along different crystal
Test or in use, the performance of alloy goes out significant difference (strong anisotropy).For example, closed for Cu-Al-Mn shape memories
Golden monocrystalline, its edge<001>The super-elasticity of orientation is up to more than 10%, and edge<111>The super-elasticity of orientation only has about 2%.
Therefore, develop controllable near<001>The preparation method of the Cu-Al-Mn marmem large size single crystals of orientation is right
In meeting application demand of the Cu-Al-Mn marmems as building, large-scale precision instrument damping energy-absorbing material
It is significant.
The content of the invention
The problem of present invention is directed to current large scale Cu-Al-Mn shape memory alloy monocrystalline tropism controls, propose to orient
Prepared by clotting method has<001>The columnar-shaped polycrystalline alloy of fiber texture degree is raw material, by controlling cycle heat treatment system and work
Skill parameter, ensure the orientation heredity in single crystal growth process, it is controllable so as to realize<001>It is prepared by the single crystal alloy of orientation.
And on the basis of above thinking, by furtheing investigate the alloy grain abnormal growth behavior of columnar-shaped polycrystalline tissue and orientation heredity
Property, suitable heat treating regime and technological parameter are developed, while realize crystal growth and tropism control.
Grown up it is an object of the invention to provide one kind based on solid grains, be controllable<001>The Cu-Al-Mn shapes of orientation
Memorial alloy method for preparing single crystal.
The present invention is achieved by the following technical solutions：
Cu-Al-Mn marmems are near<001>The preparation method of oriented single crystal, the preparation method are specifically：First
Being prepared using directional freeze method along solidification direction is had<001>The columnar-shaped polycrystalline Cu-Al-Mn marmem bases of fiber texture degree
Material, then by repeatable cycle heat treatment, make alloy β phases crystal grain that abnormal growth occur, and it is bright to keep crystal grain orientation not occur
It is aobvious to change, until water hardening when formation monocrystalline or crystallite dimension reach requirement, directly obtains or cuts out along initial solidification side
To with<001>The single crystal alloy of orientation.
Further, the composition range of the Cu-Al-Mn marmems is：Al：3at.%~20at.%, Mn：
1at.%~20at.%, remaining is Cu；
Further, the preparation method specifically includes following steps：
Step (1)：Purity is used to be above 99.9% oxygen-free copper, electrolytic aluminium and electrolytic manganese as raw material, it is solidifying using orientation
Solid method prepares Cu-Al-Mn blank of shape memory alloy；
Step (2)：Columnar-shaped polycrystalline Cu-Al-Mn blank of shape memory alloy is heated to 800~900 DEG C, insulation 10~60
Minute；
Step (3)：By alloy with the cooling velocity no more than 5 DEG C/min, 500 DEG C~600 DEG C are cooled to, insulation 10~20
Minute；
Step (4)：By step (3) alloy with the firing rate no more than 20 DEG C/min, it is again heated to 800~
900 DEG C, it is incubated 10~60 minutes；
Step (5)：As needed, repeat the above steps (3) and step (4), until forming monocrystalline or crystallite dimension reaches
It is required that when water hardening.Directly obtaining or cutting out has closely along initial solidification direction<001>The single crystal alloy of orientation；
Further, directional freeze method described in step (1) includes common directional solidification method, continuous directional solidification method etc.
The method of all achievable metal directional solidification crystallizations；
Further, the Cu-Al-Mn blank of shape memory alloy prepared described in step (1) using directional freeze method,
Have along solidification direction<001>Fiber texture degree, its alloy structure are columnar-shaped polycrystalline tissue；
Further, step (2) heat treatment process into step (4) uses inert gas shielding；
Further, the Cu-Al-Mn shape memory alloy monocrystallines at room temperature by austenite one phase or martensite single phase or
Austenite, martensite two-phase composition；
Further, it is described to obtain closely<001>Oriented single crystal refer to the initial solidification direction of monocrystal with<001>Orientation
Deviation is within 10 °.
The method have the characteristics that：The columanar structure's Cu-Al-Mn marmems prepared using directional freeze method
With edge solidification direction<001>Fiber texture degree, by controlling suitable circle heat treatment, abnormal growth mistake occurs in crystal grain
Kept in journey<001>Orientation, so as to realize the controllable Cu-Al-Mn marmem lists of the orientation based on solid-state phase changes principle
It is prepared by crystalline substance.
The advantage of the invention is that：
1. single-crystal orientation is controllable.The present invention is prepared along solidification direction with directional freeze method to be had<001>The post of fiber texture degree
The brilliant tissue strand of shape is raw material, and during cycle heat treatment, by state modulator, is ensured<001>The heredity of orientation, from
And prepared monocrystalline has closely along initial solidification direction<001>Orientation.
2. large size single crystal can be prepared.The present invention prepares alloy monocrystalline based on solid-state phase changes principle, overcomes traditional base
In the limitation that solidification principle single crystal preparation technology is difficult to prepare big chi shape memory alloy monocrystalline material；Prepared Cu-Al-Mn
Shape memory alloy monocrystalline size is up to more than 50mm.
3. technique is simple, easily operated.Compared to traditional method for preparing single crystal (such as czochralski method, Bridgeman methods), sheet
It is simple that the involved directional freeze method of invention and cycle heat treatment method are respectively provided with technique, it is easily operated the characteristics of.
Brief description of the drawings
Metallographic structure photo (a) the edge solidification side of columanar structure's Cu-Al-Mn alloys prepared by Fig. 1 directional freeze methods
To section, (b) is perpendicular to solidification direction section (SD represents solidification direction)
Crystal grain orientation inverse pole figure of Fig. 2 columanar structures Cu-Al-Mn alloys along solidification direction
Fig. 3 crystal grain orientation inverse pole figures of Cu-Al-Mn alloys along initial solidification direction after 3 cycle heat treatments
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiied
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also understand the present invention completely.
【Embodiment 1】
Using purity be 99.99% oxygen-free copper, electrolytic aluminium and electrolytic manganese as raw material, using electromagnetic induction vacuum melting system
Standby prealloy, alloying component A1：17.5at.%, Mn：11at.%, remaining is Cu, and alloy melting temp is 1300 DEG C, is protected
Temperature is air-cooled to room temperature after 20 minutes, obtain the uniform prealloy of composition.
Being prepared using directional freeze method along solidification direction is had<001>Columanar structure's sheet alloy of fiber texture degree, tool
Body technology is：By prealloy in 1150 DEG C of refuses, after insulation 20 minutes, bottom is poured into as water cooled copper mould cooling, week
(heat insulation and heating equipment is closed down after casting complete) into the graphite crystallizer of insulation (1100 DEG C of holding temperature), alloy is from bottom to top
Directional solidification, columanar structure's strand is obtained, strand size is 100mm × 20mm × 20mm.Size is cut out from strand is
50mm × 10mm × 1mm sheet material.Its macrograph is as shown in Figure 1.SD represents solidification direction in figure.
Using EBSD (EBSD, Electron Back-Scattered Diffraction) technology to post
The brilliant tissue slab of shape carries out crystal orientation analysis, and its result is as shown in Figure 2, it was demonstrated that columanar structure prepared by directional freeze method
Slab has strong along solidification direction<001>Fiber texture degree.
Columnar-shaped polycrystalline Cu-Al-Mn marmem sheet materials are heated to 900 DEG C, after being incubated 10 minutes, according to the present invention
The step carries out cycle heat treatment and (is cooled to 500 DEG C with 4 DEG C/min cooling velocity, is incubated 10 minutes, then with 10 DEG C/min
Firing rate be heated to 900 DEG C, be incubated 10 minutes, be a heat treatment cycle).During cycle heat treatment, column crystal
Abnormal growth occurs for the crystal grain of Cu-Al-Mn marmem sheet materials, but crystal grain orientation keeps constant.After 5 circulations, plate
The largest grain size of material more than 16mm × 10mm × 1mm, from prepared sheet material it is cleavable go out full-size be 16mm ×
10mm × 1mm monocrystal, crystal orientation are as shown in Figure 3.
【Embodiment 2】
Using purity be 99.99% oxygen-free copper, electrolytic aluminium and electrolytic manganese as raw material, using electromagnetic induction vacuum melting system
Standby prealloy, alloying component A1：17.5at%, Mn：11at.%, remaining is Cu, and alloy melting temp is 1200 DEG C, is protected
Temperature is air-cooled to room temperature after 20 minutes, obtain the uniform prealloy of composition.
Being prepared using directional freeze method along solidification direction is had<001>Columanar structure's sheet alloy of fiber texture degree, tool
Body technology is：By prealloy in 1150 DEG C of refuses, after insulation 20 minutes, bottom is poured into as water cooled copper mould cooling, week
(heat insulation and heating equipment is closed down after cast) into the graphite crystallizer of insulation (1100 DEG C of holding temperature), alloy from bottom to top orients
Solidification, columanar structure's strand is obtained, strand size is 100mm × 20mm × 20mm.It is 50mm that size is cut out from strand
× 10mm × 1mm sheet material.
Columnar-shaped polycrystalline Cu-Al-Mn marmem sheet materials are heated to 900 DEG C, after being incubated 30 minutes, according to the present invention
The step carries out cycle heat treatment and (is cooled to 500 DEG C with 3 DEG C/min cooling velocity, is incubated 30 minutes, then with 15 DEG C/min
Firing rate be heated to 900 DEG C, be incubated 30 minutes, be a heat treatment cycle).After 10 circulations, single crystal alloy is obtained
Sheet material.
【Embodiment 3】
Using purity be 99.99% oxygen-free copper, electrolytic aluminium and electrolytic manganese as raw material, using electromagnetic induction vacuum melting system
Standby prealloy, alloying component A1：17at%, Mn：11at.%, remaining is Cu, and alloy melting temp is 1200 DEG C, insulation
Room temperature is air-cooled to after 20 minutes, obtains the uniform prealloy of composition.
Being prepared using continuous directional solidification method along solidification direction is had<001>Columanar structure's alloy bar of fiber texture degree
Material, concrete technology are：Using pull-down continuous directional solidification apparatus, first by prealloy in 1200 DEG C of refuses, control
Graphite casting mould temperature is 1100 DEG C, casting speed 20mm/min.It is 10mm to prepare diameter of rod.Intercepted length is 100mm
Bar.
Columnar-shaped polycrystalline Cu-Al-Mn shape memory alloy bar materials are heated to 900 DEG C, after being incubated 30 minutes, according to the present invention
The step carries out cycle heat treatment and (is cooled to 500 DEG C with 3 DEG C/min cooling velocity, is incubated 30 minutes, then with 12 °C/min
Firing rate be heated to 850 DEG C, be incubated 30 minutes, be a heat treatment cycle).After 12 circulations, single crystal alloy is obtained
Bar.
Claims (7)
- A kind of 1. preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines, it is characterised in that the preparation method The edge solidification direction prepared with directional freeze method has<001>The columnar-shaped polycrystalline Cu-Al-Mn marmems of fiber texture degree are Raw material, using cycle heat treatment method, make alloy grain that continuous abnormal occur and grow up, realize crystal growth；Meanwhile pass through control Cycle heat treatment system, ensure that crystal grain orientation does not occur substantially to change in single crystal growth process, so as to obtain along initial solidification side To near<001>The Cu-Al-Mn shape memory alloy monocrystallines of orientation, the composition model of the Cu-Al-Mn marmems Enclose for：Al：3at.%~20at.%, Mn：1at.%~20at.%, remaining is Cu.
- 2. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 1, its feature It is, comprises the following steps that：Step (1)：Purity is used to be above 99.9% oxygen-free copper, electrolytic aluminium and electrolytic manganese as raw material, using directional solidification side Method prepares Cu-Al-Mn blank of shape memory alloy；Step (2)：Columnar-shaped polycrystalline Cu-Al-Mn blank of shape memory alloy is heated to 800~900 DEG C, is incubated 10~60 points Clock；Step (3)：By alloy with the cooling velocity no more than 5 DEG C/min, 500 DEG C~600 DEG C are cooled to, is incubated 10~20 points Clock；Step (4)：By step (3) alloy with the firing rate no more than 20 DEG C/min, 800~900 DEG C are again heated to, Insulation 10~60 minutes；Step (5)：As needed, (the 3)~step that repeats the above steps (4), until formation monocrystalline or crystallite dimension reach requirement, Then water hardening, directly obtaining or cutting out has closely along initial solidification direction<001>The single crystal samples of orientation.
- 3. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 2, its feature It is, directional freeze method described in step (1) includes common directional solidification method, all achievable metals of continuous directional solidification method The method of directional solidification crystallization.
- 4. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 2, its feature It is, the Cu-Al-Mn blank of shape memory alloy prepared described in step (1) using directional freeze method, its microstructure is Have along solidification direction<001>The columnar-shaped polycrystalline tissue of fiber texture degree.
- 5. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 2, its feature It is, the heat treatment process of step (2) to step (4) uses inert atmosphere protection.
- 6. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 2, its feature It is, the single crystal alloy of preparation is made up of austenite one phase or martensite single phase or austenite, martensite two-phase at room temperature.
- 7. a kind of preparation method for being orientated controllable Cu-Al-Mn shape memory alloy monocrystallines according to claim 2, its feature It is, it is described to obtain closely<001>Oriented single crystal refer to the initial solidification direction of monocrystal with<001>The deviation of orientation 10 ° with It is interior.
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| CN109112349A (en) * | 2018-10-25 | 2019-01-01 | 哈尔滨工程大学 | A kind of CuAlMn marmem and preparation method thereof |
| CN109338452A (en) * | 2018-12-06 | 2019-02-15 | 重庆科技学院 | A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline |
| CN109457091A (en) * | 2018-10-15 | 2019-03-12 | 四川大学 | A method of preparing coarse-grain Fe-Mn-Si base marmem |
| CN112195422A (en) * | 2020-09-11 | 2021-01-08 | 中铝材料应用研究院有限公司 | Preparation method of single-crystal-like pure copper |
| CN113373342A (en) * | 2021-05-28 | 2021-09-10 | 上海理工大学 | Preparation method of high-superelasticity CuAlMn shape memory alloy wire |
| CN113846244A (en) * | 2021-09-20 | 2021-12-28 | 哈尔滨工程大学 | CuAlMn shape memory alloy and preparation method thereof |
| CN114182352A (en) * | 2021-12-13 | 2022-03-15 | 西北工业大学 | Preparation method of multi-stage directional growth metal material under multi-field action |
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Cited By (10)
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| CN109457091A (en) * | 2018-10-15 | 2019-03-12 | 四川大学 | A method of preparing coarse-grain Fe-Mn-Si base marmem |
| CN109112349A (en) * | 2018-10-25 | 2019-01-01 | 哈尔滨工程大学 | A kind of CuAlMn marmem and preparation method thereof |
| CN109338452A (en) * | 2018-12-06 | 2019-02-15 | 重庆科技学院 | A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline |
| CN112195422A (en) * | 2020-09-11 | 2021-01-08 | 中铝材料应用研究院有限公司 | Preparation method of single-crystal-like pure copper |
| CN113373342A (en) * | 2021-05-28 | 2021-09-10 | 上海理工大学 | Preparation method of high-superelasticity CuAlMn shape memory alloy wire |
| CN113373342B (en) * | 2021-05-28 | 2022-07-22 | 上海理工大学 | Preparation method of high-superelasticity CuAlMn shape memory alloy wire |
| CN113846244A (en) * | 2021-09-20 | 2021-12-28 | 哈尔滨工程大学 | CuAlMn shape memory alloy and preparation method thereof |
| CN113846244B (en) * | 2021-09-20 | 2022-06-21 | 哈尔滨工程大学 | CuAlMn shape memory alloy and preparation method thereof |
| CN114182352A (en) * | 2021-12-13 | 2022-03-15 | 西北工业大学 | Preparation method of multi-stage directional growth metal material under multi-field action |
| CN114182352B (en) * | 2021-12-13 | 2023-01-17 | 西北工业大学 | Preparation method of multi-stage directional growth metal material under multi-field action |
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