CN109338452A - A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline - Google Patents
A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline Download PDFInfo
- Publication number
- CN109338452A CN109338452A CN201811489324.0A CN201811489324A CN109338452A CN 109338452 A CN109338452 A CN 109338452A CN 201811489324 A CN201811489324 A CN 201811489324A CN 109338452 A CN109338452 A CN 109338452A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- magnesium alloy
- heat
- heat treatment
- large scale
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- 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
- C30B29/52—Alloys
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Sampling And Sample Adjustment (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses the method for a kind of heat treating process preparation large scale magnesium or magnesium alloy monocrystalline, include the steps that magnesium or magnesium alloy carrying out level Four heat treatment.The present invention has prepared large-sized magnesium or magnesium alloy monocrystalline with reasonable heat treatment process, and preparation process of the invention is simple, it is low in cost, the magnesium or magnesium alloy monocrystalline of large scale (several centimetres to number meter ruler cun) can be prepared in the case where heating furnace size allows.
Description
Technical field
The invention belongs to magnesium and Magnesium alloy AZ91D fields, and in particular to the preparation side of a kind of magnesium or magnesium alloy monocrystalline
Method.
Background technique
Magnesium and magnesium alloy are structural materials most light in practical metal, and it is the 1/4 of iron that specific gravity, which is the 2/3 of aluminium,.In addition, magnesium
Alloy has the excellent properties such as shock resistance is strong, wearability and thermal conductivity are excellent, waste material easily recycles, in aerospace, automobile, electricity
Son, instrument and meter industry have obtained wide application.Compared to polycrystalline magnesium material, monocrystalline magnesium have better mechanical property and
Electrical properties, with the development of opto-electronics and wireless telecommunications, magnesium monocrystalline possesses vast market prospect.In addition, utilizing magnesium list
Crystalline substance carries out related basic research, and a spotlight of magnesium research at present, and therefore, public at present there is an urgent need to a kind of economical and effectives
Magnesium single crystal preparation technique.
According to literature research status both domestic and external, at present the preparation method of magnesium monocrystalline mainly have directional solidification method and focus from
Beamlet method.Directional solidification method includes dry pot descent method, segmented heat preservation etc., and principle is the induction melting material in monocrystal growing furnace
Directional solidification, preparation process are affected by cooling velocity, alloying component, level of vacuum etc., in the sample of preparation often at
Divide segregation, grain size is also difficult to control.It is mostly micro- cylinder (tens microns) that focused ion beam (FIB) method, which prepares sample, though
Monocrystalline quality, but higher cost can be so controlled, it is small-sized.
In conclusion limited at present by technical conditions, the technology of preparing of magnesium and magnesium alloy monocrystalline mostly by special installation,
Preparation process is affected by many factors, inconvenient, and the magnesium single crystal size prepared is also limited.Therefore, seek a kind of letter
Single, economical and effective large scale magnesium and magnesium alloy method for preparing single crystal are the important classes of Study for Magnesium Composites and industrial application
Topic.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of large scale magnesium of simple economy or magnesium alloy single crystal preparation sides
Method.
In order to achieve the above objectives, the invention provides the following technical scheme:
A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline, comprising the following steps:
(1) first order is heat-treated: magnesium or magnesium alloy are kept the temperature 5-20h at 200-420 DEG C；
(2) second level is heat-treated: by the magnesium after step (1) first order is heat-treated or magnesium alloy at 300-450 DEG C
Keep the temperature 48-150h；
(3) third level is heat-treated: by the magnesium after step (2) second level is heat-treated or magnesium alloy at 400-550 DEG C
Keep the temperature 20-90h；
(4) fourth stage is heat-treated: by the magnesium after step (3) third level is heat-treated or magnesium alloy at 450-600 DEG C
Keep the temperature 20-90h.
As currently preferred technical solution, in the step (1), the temperature of first order heat treatment is 300-400 DEG C,
Soaking time is 10-16h.
As currently preferred technical solution, in the step (2), the temperature of second level heat treatment is 300-400 DEG C,
Soaking time is 60-120h.
As currently preferred technical solution, in the step (3), the temperature of third level heat treatment is 450-550 DEG C,
Soaking time is 30-60h.
As currently preferred technical solution, in the step (4), the temperature of fourth stage heat treatment is 480-570 DEG C,
Soaking time is 30-60h.
Currently preferred technical solution heat treatment duration is shorter or energy consumption is lower.
In the inventive solutions, there are two types of selections for the bridging mode between heat treatments at different levels: a kind of mode is to connect
Continuous uninterrupted progress, after the completion of upper level heat treatment heat preservation, direct alternating temperature enters next stage heat treatment；Another way is interruption
It carries out, after every grade of heat treatment, magnesium or magnesium alloy is taken out into cooling, then carry out next stage heat treatment.Of course, it is possible to select routine
The type of cooling, such as natural cooling in air.
In the inventive solutions, when being heat-treated to the temperature and heat preservation of fourth stage heat treatment for the first order
Between, those skilled in the art are can be according to the size adjusting of magnesium or magnesium alloy, for large-sized magnesium or magnesium alloy, it should
Properly increase heat treatment temperature and/or soaking time.
In the inventive solutions, the object of processing can be pure magnesium or AZ31, AZ61, AZ80, AZ91, AM50,
The magnesium alloy of the various trades mark such as ZK60.
In the inventive solutions, it is each to can be casting and forming, roll forming or extrusion forming etc. for the object of processing
The magnesium of magnesium or magnesium alloy plate, tubing, bar, profile, band that kind of forming method obtains etc., preferably rolling or extrusion forming or
Magnesium alloy plate.
The beneficial effects of the present invention are:
The present invention has prepared large-sized magnesium or magnesium alloy monocrystalline, and system of the invention with reasonable heat treatment process
Standby simple process and low cost can prepare (several centimetres to number meter ruler of large scale in the case where heating furnace size allows
It is very little) magnesium or magnesium alloy monocrystalline.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the micro-organization chart of the Sample A of embodiment 1 before heat treatment；
Fig. 2 is microscopic structure spliced map of the Sample A of embodiment 1 after fourth stage heat treatment；
Fig. 3 is micro-organization chart of the Sample A of embodiment 1 after fourth stage heat treatment under high-amplification-factor；
Fig. 4 is micro-organization chart of the sample B of embodiment 2 after fourth stage heat treatment；
Fig. 5 is micro-organization chart of the sample C of embodiment 3 after fourth stage heat treatment.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It better understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1:
Sample A is size 0.8mm × 55mm × 35mm AZ31 magnesium alloy plate.
Fig. 1 is the micro-organization chart of Sample A before heat treatment, and sample tissue is the irregular polycrystalline material in grain boundary.
First order heat treatment: keeping the temperature 12h at 400 DEG C for Sample A, eliminate material part internal stress, then takes out in air certainly
It is so cooling.Second level heat treatment: Sample A is kept the temperature into 60h at 450 DEG C, then takes out natural cooling in air.Third level heat
Processing: Sample A is kept the temperature into 48h at 500 DEG C, then takes out natural cooling in air.Fourth stage heat treatment: Sample A is existed
50h is kept the temperature at 530 DEG C, then takes out natural cooling in air.Fig. 2 is microscopic structure of the Sample A after fourth stage heat treatment
Spliced map, magnesium alloy successfully grow into one block of large scale magnesium alloy monocrystalline for being about 35mm, width about 55mm.Fig. 3 is Sample A the
Micro-organization chart after level Four heat treatment under high-amplification-factor.
Embodiment 2:
Sample B is size 0.8mm × 55mm × 52mm AZ31 magnesium alloy plate.
Sample B has carried out level Four heat treatment altogether.First order heat treatment: sample B 20h, heat preservation in 200 DEG C of heating furnaces terminate
Second level heat treatment is directly carried out afterwards.Second level heat treatment: sample B keeps the temperature 120h at 300 DEG C, directly carries out after heat preservation
Third level heat treatment.Third level heat treatment: sample B keeps the temperature 60h at 400 DEG C.It is directly carried out at fourth stage heat after heat preservation
Reason.Fourth stage heat treatment: sample B keeps the temperature 84h at 450 DEG C.Fig. 4 is micro-organization chart of the sample B after fourth stage heat treatment,
Sample B tissue does not find that crystal boundary, magnesium plate tissue are monocrystalline.
Embodiment 3:
Sample C is size 0.8mm × 55mm × 71mm AZ31 magnesium alloy plate.
Sample C has carried out level Four heat treatment altogether.First order heat treatment: sample C 10h, heat preservation in 350 DEG C of heating furnaces terminate
It is air-cooled afterwards.Second level heat treatment: sample C keeps the temperature 72h at 400 DEG C, and cooling is taken out after heat preservation.Third level heat treatment: examination
Sample C keeps the temperature 20h at 520 DEG C, and cooling is taken out after heat preservation.Fourth stage heat treatment: sample C keeps the temperature 20h at 550 DEG C.Fig. 5
For micro-organization chart of the sample C after fourth stage heat treatment, magnesium plate tissue is monocrystalline.
The present invention is in practicing, when being heat-treated to the temperature and heat preservation of fourth stage heat treatment for the first order
Between, those skilled in the art are can be according to the size adjusting of magnesium or magnesium alloy, for large-sized magnesium or magnesium alloy, it should
Properly increase heat treatment temperature and/or soaking time.
Under normal conditions, it is 200-400 DEG C that the first order, which is heat-treated more appropriate heat treatment temperature, soaking time 5-
20h, preferred heat treatment temperature are 300-400 DEG C, soaking time 10-16h；The second level is heat-treated more appropriate heat treatment
Temperature is 300-450 DEG C, soaking time 48-150h, and preferred heat treatment temperature is 300-400 DEG C, soaking time 60-
120h；It is 400-550 DEG C, soaking time 20-90h that the third level, which is heat-treated more appropriate heat treatment temperature, at preferred heat
Managing temperature is 450-550 DEG C, soaking time 30-60h；It is 450-600 that the fourth stage, which is heat-treated more appropriate heat treatment temperature,
DEG C, soaking time 20-90h, preferred heat treatment temperature is 480-570 DEG C, soaking time 30-60h.But this technology
The technical staff in field made equivalent substitute or transformation in above-mentioned heat treatment temperature and soaking time, in guarantor of the invention
Within the scope of shield.
The present invention is in practicing, and there are two types of selections for bridging mode between heat treatments at different levels: a kind of mode is continuous
Uninterrupted to carry out, after the completion of upper level heat treatment heat preservation, direct alternating temperature enters next stage heat treatment；Another way be interrupted into
Magnesium or magnesium alloy are taken out cooling, then carry out next stage heat treatment after every grade of heat treatment by row；Of course, it is possible to select conventional
The type of cooling, such as natural cooling in air.It should be appreciated by those skilled in the art that above two mode can reach this hair
Bright purpose, it is within the scope of the present invention.
Those skilled in the art are it should be understood that in the inventive solutions, the object of processing can be pure
The magnesium alloy of the various trades mark such as magnesium or AZ31, AZ61, AZ80, AZ91, AM60, ZK60.
Those skilled in the art are it should be understood that in the inventive solutions, the object of processing can be casting
The magnesium or magnesium alloy plate, tubing, bar, profile, band for causing the various forming methods such as type, roll forming or extrusion forming to obtain
Material etc..
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of method of heat treating process preparation large scale magnesium or magnesium alloy monocrystalline, it is characterised in that: the following steps are included:
(1) first order is heat-treated: magnesium or magnesium alloy are kept the temperature 5-20h at 200-420 DEG C；
(2) second level be heat-treated: by by step (1) first order be heat-treated after magnesium or magnesium alloy kept the temperature at 300-450 DEG C
48-150h；
(3) third level be heat-treated: by by step (2) second level be heat-treated after magnesium or magnesium alloy kept the temperature at 400-550 DEG C
20-90h；
(4) fourth stage be heat-treated: by by step (3) third level be heat-treated after magnesium or magnesium alloy kept the temperature at 450-600 DEG C
20-90h。
2. the method for heat treating process preparation large scale magnesium according to claim 1 or magnesium alloy monocrystalline, it is characterised in that: institute
It states in step (1), the temperature of first order heat treatment is 300-400 DEG C, soaking time 10-16h.
3. the method for heat treating process preparation large scale magnesium according to claim 1 or magnesium alloy monocrystalline, it is characterised in that: institute
It states in step (2), the temperature of second level heat treatment is 300-400 DEG C, soaking time 60-120h.
4. the method for heat treating process preparation large scale magnesium according to claim 1 or magnesium alloy monocrystalline, it is characterised in that: institute
It states in step (3), the temperature of third level heat treatment is 450-550 DEG C, soaking time 30-60h.
5. the method for heat treating process preparation large scale magnesium according to claim 1 or magnesium alloy monocrystalline, it is characterised in that: institute
It states in step (4), the temperature of fourth stage heat treatment is 480-570 DEG C, soaking time 30-60h.
6. according to claim 1 to the method that heat treating process described in 5 any one prepares large scale magnesium or magnesium alloy monocrystalline,
It is characterized in that: after every grade of heat treatment, magnesium or magnesium alloy being taken out into cooling, then carry out next stage heat treatment.
7. the method for heat treating process preparation large scale magnesium according to claim 6 or magnesium alloy monocrystalline, it is characterised in that: institute
Cooling mode is stated as natural cooling in air.
8. according to claim 1 to the method that heat treating process described in 5 any one prepares large scale magnesium or magnesium alloy monocrystalline,
Be characterized in that: the temperature and soaking time that the first order is heat-treated to fourth stage heat treatment are according to magnesium or the size tune of magnesium alloy
It is whole.
9. the method for heat treating process preparation large scale magnesium according to claim 1 or magnesium alloy monocrystalline, it is characterised in that: institute
It states magnesium or magnesium alloy is magnesium or magnesium alloy plate.
10. the method for heat treating process preparation large scale magnesium according to claim 9 or magnesium alloy monocrystalline, it is characterised in that:
The magnesium or magnesium alloy plate are the magnesium or magnesium alloy plate of rolling or extrusion forming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811489324.0A CN109338452B (en) | 2018-12-06 | 2018-12-06 | Method for preparing large-size magnesium or magnesium alloy single crystal by heat treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811489324.0A CN109338452B (en) | 2018-12-06 | 2018-12-06 | Method for preparing large-size magnesium or magnesium alloy single crystal by heat treatment method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109338452A true CN109338452A (en) | 2019-02-15 |
| CN109338452B CN109338452B (en) | 2021-03-30 |
Family
ID=65297411
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811489324.0A Active CN109338452B (en) | 2018-12-06 | 2018-12-06 | Method for preparing large-size magnesium or magnesium alloy single crystal by heat treatment method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109338452B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6461394A (en) * | 1987-08-31 | 1989-03-08 | Nippon Mining Co | Production of molybdenum single crystal |
| CN101191168A (en) * | 2006-11-23 | 2008-06-04 | 北京有色金属研究总院 | Magnesium alloy and preparation method thereof |
| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN104404614A (en) * | 2014-12-29 | 2015-03-11 | 中南大学 | Preparation method of Al-Cu-Mg aluminum alloy monocrystal |
| CN105714382A (en) * | 2016-02-23 | 2016-06-29 | 北京大学 | Preparation method of large-size Cu(100) single-crystal copper foil |
| CN107841790A (en) * | 2017-10-20 | 2018-03-27 | 北京科技大学 | A kind of preparation method for being orientated controllable Cu Al Mn shape memory alloy monocrystallines |
-
2018
- 2018-12-06 CN CN201811489324.0A patent/CN109338452B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6461394A (en) * | 1987-08-31 | 1989-03-08 | Nippon Mining Co | Production of molybdenum single crystal |
| CN101191168A (en) * | 2006-11-23 | 2008-06-04 | 北京有色金属研究总院 | Magnesium alloy and preparation method thereof |
| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN104404614A (en) * | 2014-12-29 | 2015-03-11 | 中南大学 | Preparation method of Al-Cu-Mg aluminum alloy monocrystal |
| CN105714382A (en) * | 2016-02-23 | 2016-06-29 | 北京大学 | Preparation method of large-size Cu(100) single-crystal copper foil |
| CN107841790A (en) * | 2017-10-20 | 2018-03-27 | 北京科技大学 | A kind of preparation method for being orientated controllable Cu Al Mn shape memory alloy monocrystallines |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109338452B (en) | 2021-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Comparison of microstructures and mechanical properties of Inconel 718 alloy processed by selective laser melting and casting | |
| Jiang et al. | Microstructure and texture evolution of the cold-rolled AZ91 magnesium alloy strip under electropulsing treatment | |
| Zhang et al. | Grain refinement in highly undercooled solidification of Ni85Cu15 alloy melt: Direct evidence for recrystallization mechanism | |
| Black et al. | Optimizing seeded casting of mono-like silicon crystals through numerical simulation | |
| Stanford et al. | Seeding of single crystal superalloys––role of seed melt-back on casting defects | |
| Meng et al. | Effect of platform dimension on the dendrite growth and stray grain formation in a Ni-base single-crystal superalloy | |
| CN107541627B (en) | A kind of wrought magnesium alloy plate and preparation method thereof with good room temperature formability | |
| Pang et al. | Hot deformation behavior and microstructure evolution of Mg-Gd-Y (-Sm)-Zr alloys | |
| CN109161770A (en) | A kind of high-modulus magnesium alloy and preparation method thereof | |
| CN104328501B (en) | Fully controllable TiAl single crystal alloys of a kind of lamellar orientation and preparation method thereof | |
| CN102672150A (en) | Direct control method for titanium-aluminum-niobium alloy lamellar structure | |
| CN104651764A (en) | Solid solution thermal treatment method for high-zinc scandium-containing aluminum alloy | |
| CN104878452A (en) | High-temperature high-strength TiAl-Nb monocrystal and preparation method thereof | |
| CN111575619B (en) | Method for rapidly eliminating dendrite segregation in deformed high-temperature alloy ingot by pulse current | |
| CN109023180A (en) | The ageing hot processing method of 7 line aluminium alloys | |
| Zhang et al. | Single crystal growth and magnetic properties of 2: 17-type SmCo magnets | |
| CN109576543A (en) | A method of improving magnesium alloy long-time service life using baking | |
| Ai et al. | Misorientation induced by withdrawal rate transition and its effect on intermediate temperature stress rupture properties of a Ni3Al based single crystal superalloy | |
| CN103305736B (en) | MgLiAlSrY alloy and preparation method thereof | |
| Li et al. | Effect of a high magnetic field on the morphological instability and irregularity of the interface of a binary alloy during directional solidification | |
| Ge et al. | Achievement of forging without canning for β-solidifying γ-TiAl alloy containing high content of niobium | |
| CN109338452A (en) | A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline | |
| Huang et al. | Nonuniform recrystallization and growth behavior of β grains dominated by grain misorientation and interfacial energy in metastable β titanium alloy | |
| CN106350756B (en) | A kind of homogenization heat treatment method of magnesium-rare earth casting | |
| CN110358963B (en) | FeMnAlNi shape memory alloy and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |