CN108677050A - A kind of preparation method of porous magnetic memorial alloy - Google Patents
A kind of preparation method of porous magnetic memorial alloy Download PDFInfo
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- CN108677050A CN108677050A CN201810510957.9A CN201810510957A CN108677050A CN 108677050 A CN108677050 A CN 108677050A CN 201810510957 A CN201810510957 A CN 201810510957A CN 108677050 A CN108677050 A CN 108677050A
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- memorial alloy
- magnetic memorial
- porous magnetic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The present invention is to provide a kind of preparation methods of porous magnetic memorial alloy.Metal powder granulates by magnetic memorial alloy particle of the particle size less than 50 microns with particle size less than 50 microns are according to product than being 1：0.7~1.5 ratio carries out dispensing mixing；Then 30~60 minutes high-speed stirreds are carried out using ball mill to mix；By mixed powder, bulk is made in cold moudling at room temperature, and pressure is 700~800MPa；The bulk of cold moudling is placed in sinter molding in tube furnace, sinter molding temperature is 850~900 DEG C, and soaking time is 20~60 minutes, is protected using flowing argon gas, removes metal-powder by high temperature sintering, obtains porous magnetic memorial alloy bulk.Compared with common template casting, this method has many advantages, such as that simple for process, forming temperature is low, manufacturing cost is low, favorable repeatability.
Description
Technical field
The present invention relates to a kind of preparation methods of porous alloy, specifically a kind of to have martensitic traoformation
The preparation method of the porous magnetic memorial alloy of characteristic.
Background technology
Magnetic memorial alloy has both ferromagnetism and thermoelastic martensitic transformation, shows big magneto-strain and response frequency
Rate is a kind of intellectual material with good development prospect.The monocrystalline NiMnGa magnetic memorial alloy magnetic reported at present, which induces, to be become
Up to 6~10%, it is much larger than the magneto-strain (0.1~0.2%) of giant magnetostrictive material Terfenol-D, has work substantially
Journey application value.Compared with conventional temperature control NiTi marmems (response frequency is~Hz), magnetic memorial alloy can lead to
Magnetic field control is crossed, therefore there is higher response frequency (~KHz).Based on the unique functional characteristic of magnetic memorial alloy, it is expected to
For making novel energy converter, driver, sensing element, damper etc., have broad application prospects.Magnetic memorial alloy master
To include the series alloys such as NiMnGa, NiFeGa, FePt, FePd and NiMnX (X=In, Sb, Sn).The excellent magnetic reported at present
It causes strain property to mostly come from single crystal alloy, but is had the following problems when single crystal alloy preparation：Serious component segregation, again
Renaturation and stability are poor, it is difficult, with high costs to prepare.In contrast, polycrystalline material is easy to prepare, throughput rate is high and at low cost
It is honest and clean, but for polycrystal, a large amount of crystal boundary seriously inhibits twin boundary migration, leads to the magneto-strain very little or several of polycrystalline alloy
It is zero, and brittleness is big.These disadvantages seriously hinder the application and development of magnetic memorial alloy.
The researcher of the problem of for polycrystalline alloy, Northwestern Univ USA and Boise university proposes preparation
Magnetic memorial alloy foam, it is quasi- to reduce the influence that crystal boundary moves martensitic twin circle by introducing porous structure.Experimental study
Show that the introducing of porous structure can substantially reduce number of grain boundaries, to reduce the constraint that crystal boundary moves martensitic twin circle,
The maximum magneto-strain that they have suffered report in NiMnGa foamed materials is up to 8.7%, already close to the mangneto of single crystal alloy
Strain value.Therefore, porous alloy has both the advantages of polycrystalline alloy preparation is easy, cost is relatively low and single crystal alloy large magneto-strain,
It is the important directions of the following magnetic memorial alloy development.Porous material obtained in engineering practice at present it is commonly used,
Play a part of structure, buffering, damping, heat-insulated, noise reduction, filtering.It is dual that porous metal material is that one kind having both function and structure
The engineering material of attribute, have low bulk density, large specific surface area, energy-absorbing damping, sound-deadening and noise-reducing, electromagnetic shielding, air-and water-permeable,
The characteristics such as lower thermal conductivity.Therefore, porous magnetic memorial alloy is in addition to the characteristics such as magneto-strain and memory effect, also having it
The advantages of its porous metal material, thus it is multi-field with vast potential for future development in vibration damping, driving, sensing and shielding etc..
What the porous magnetic memorial alloy preparation of American researcher's report mainly utilized is template casting
(replication casting), prepares porous preform using high-melting-point inorganic salts as raw material sintering first, then utilizes height
Body of calming the anger in the magnetic memorial alloy of melting indentation porous preform, will add the method for sonic oscillation by nothing using strong acid after molding
Machine salt precast body removes, and obtains porous magnetic memorial alloy.This method preparation process is complicated, due to needing magnetic memorial alloy
Be pressed into precast body after melting, thus forming temperature it is high (>1200℃).In addition, can be different degrees of when removing precast body using pickling
Corrode magnetic memorial alloy, while sonic oscillation process easily makes alloy generate many tiny micro-cracks, makes porous memorial alloy rib
Column surface generates defect, to have an adverse effect to the stability of alloy property.
Invention content
The purpose of the present invention is to provide a kind of porous magnetics simple for process, forming temperature is low, production efficiency is high, at low cost
The preparation method of property memorial alloy.
The object of the present invention is achieved like this：
Metal powder by magnetic memorial alloy particle of the particle size less than 50 microns with particle size less than 50 microns
Particle is according to product than being 1：0.7~1.5 ratio carries out dispensing mixing；Then 30~60 minutes high-speed stirrings are carried out using ball mill
Mix mixing；By mixed powder, bulk is made in cold moudling at room temperature, and pressure is 700~800MPa；By cold moudling
Bulk is placed in sinter molding in tube furnace, and sinter molding temperature is 850~900 DEG C, and soaking time is 20~60 minutes, utilizes stream
Dynamic argon gas is protected, and is removed metal-powder by high temperature sintering, is obtained porous magnetic memorial alloy bulk.
The present invention can also include：
1. magnetic memorial alloy particle described in is NiMnGa or NiCoMnIn.
2. metal powder granulates described in are spheric granules magnesium powder.
3. controlling porosity by changing metal powder granulates content.
The porous magnetic memorial alloy of the present invention once sintered can be molded, can be with control hole by changing metal powder content
Gap rate.Compared with common template casting, this method is with simple for process, forming temperature is low, manufacturing cost is low, repeatable
The advantages that good.Main advantages of the present invention are embodied in：
(1) preparation method of the invention, which reduces template casting and prepares porous magnetic memorial alloy, needs Prefabricated porous pre-
The step of body processed and follow-up removal precast body, therefore simple for process, can quickly once sintered molding, production efficiency is high；In addition,
Due to need not melt magnetic memorial alloy, forming temperature is low, can effectively reduce manufacturing cost.
(2) the invention avoids generate corrosion to alloy when template casting removes precast body by pickling and ultrasonic vibration
With the adverse effects such as micro-crack；
(3) present invention can obtain the porous magnetic memorial alloy of different porosities by simply controlling metal powder content
Bulk.
Description of the drawings
Fig. 1 is the preparation process schematic diagram of porous magnetic memorial alloy；
Fig. 2 (a)-Fig. 2 (b) is the optical microscope photograph of porous NiMnGa magnetic memorial alloys, wherein：Fig. 2 (a) is vertical
The plane in direct-cooled pressure direction, Fig. 2 (b) are the plane in parallel cold pressing direction.
Fig. 3 (a)-Fig. 3 (b) is the back scattering stereoscan photograph of porous NiMnGa magnetic memorial alloys, wherein：Fig. 3 (a)
To be vertically cold-pressed direction plane, Fig. 3 (b) is the plane in parallel cold pressing direction, it can be seen that the predominantly through-hole knot formed
Structure
Fig. 4 is the Fracture scan electromicroscopic photograph of porous NiMnGa magnetic memorial alloys, and as can be seen from the figure hole is closing
Golden internal formed is uniformly distributed.
Fig. 5 is ac magnetic susceptibility-temperature test curve of porous NiMnGa magnetic memorial alloys, and alloy is in -20 DEG C and 30
Martensitic traoformation (A → M) and reverse transformation (M → A) have occurred between DEG C, Curie transition (T occurs at~70 DEG CC)。
Fig. 6 (a)-Fig. 6 (d) is the optical microscope photograph of porous NiCoMnIn magnetic memorial alloys, wherein：Fig. 6 (a),
Fig. 6 (b) is the plane in vertical cold pressing direction, and Fig. 6 (c), Fig. 6 (d) are the plane in parallel cold pressing direction, as can be observed from Figure
Apparent martensite lath illustrates porous NiCoMnIn magnetic memorial alloys in room temperature based on martensitic phase.
Fig. 7 (a)-Fig. 7 (b) is the back scattering stereoscan photograph of porous NiCoMnIn magnetic memorial alloys, wherein：Fig. 7
(a) it is the vertical plane for being cold-pressed direction, Fig. 7 (b) is the plane in parallel cold pressing direction, therefrom it can be seen that the hole that alloy is formed
Distribution is more uniform.
Specific implementation mode
The basic step that the present invention prepares porous magnetic memorial alloy using sintering process is：
(1) selection particle size is less than 50 microns of magnetic memorial alloy particle；(2) selection particle size is less than 50 microns
Metal powder granulates；(3) by magnetic memorial alloy powder and metal powder by volume 1：(0.7~1.5) it is mixed to carry out dispensing
It closes, then carrying out 30~60 minutes high-speed stirreds using ball mill mixes；(4) by mixed-powder cold moudling at room temperature, pressure
Power is 700~800MPa, and bulk is made；(5) cold moudling sample is placed in sinter molding in tube furnace, forming temperature 850
~900 DEG C, soaking time is 20~60 minutes, is protected using flowing argon gas, removes metal-powder by high temperature sintering, obtains
Obtain porous magnetic memorial alloy bulk.
It illustrates below and the present invention is described in more detail.
Specific embodiment 1
It is prepared by NiMnGa porous magnetic memorial alloys：(1) it utilizes public in patent No. ZL200710071687.8 patent documents
The high-energy ball milling method opened prepares Ni49.8Mn28.5Ga21.7Magnetic memorial alloy particle obtains particle size and is less than 50 microns
NiMnGa particles；(2) ball-shaped magnesite powder (atomization molding) of the selection particle size less than 50 microns；(3) by NiMnGa alloy powders
With magnesium powder by volume 1：1 carries out mixed powder in high speed ball mill, and the time is 30 minutes；(4) mixed powder is placed in mould
In tool cylindrical block is cold-pressed under 770MPa pressure；(5) will be molded bulk be put into be connected with flowing argon gas tube furnace in into
Row sintering is heated to 900 DEG C from room temperature with 5 DEG C/min, keeps the temperature 1 hour, cool to 200 DEG C with 5 DEG C/min, then furnace cooling
To room temperature, NiMnGa porous magnetic memorial alloys are obtained.The microstructure picture of porous alloy such as Fig. 2 (a)-Fig. 2 (b), Fig. 3
(a) shown in-Fig. 3 (b)；Its fracture apperance is as shown in Figure 4；The curved line relation of ac magnetic susceptibility and temperature is as shown in figure 5, show to obtain
The NiMnGa porous magnetic memorial alloys obtained have martensitic traoformation characteristic.
Specific embodiment 2
It is prepared by NiCoMnIn porous magnetic memorial alloys：(1) it utilizes in patent No. ZL200710071687.8 patent documents
Disclosed high-energy ball milling method prepares Ni45Co5Mn36.7In13.3Magnetic memorial alloy particle obtains particle size and is less than 50 microns
NiCoMnIn particles；(2) ball-shaped magnesite powder (atomization molding) of the selection particle size less than 50 microns；(3) by NiCoMnIn alloys
Powder and magnesium powder by volume 1：1 carries out mixed powder in high speed ball mill, and the time is 30 minutes；(4) mixed powder is set
In mold cylindrical block is cold-pressed under 770MPa pressure；(5) bulk is put into be connected with flowing argon gas tube furnace in into
Row sintering is heated to 900 DEG C from room temperature with 5 DEG C/min, keeps the temperature 1 hour, cool to 200 DEG C with 5 DEG C/min, then furnace cooling
To room temperature, NiCoMnIn porous magnetic memorial alloys are obtained.The microstructure picture of porous alloy such as Fig. 6 (a)-Fig. 6 (d), Fig. 7
(a) shown in-Fig. 7 (b), martensite lath can be obviously observed from optical photograph, illustrates that alloy is mainly with geneva at room temperature
Based on body phase.
Claims (5)
1. a kind of preparation method of porous magnetic memorial alloy, it is characterized in that：Particle size is less than to 50 microns of Magnetic memory
Metal powder granulates of the alloying pellet with particle size less than 50 microns are according to product than being 1：0.7~1.5 ratio carries out dispensing
Mixing；Then 30~60 minutes high-speed stirreds are carried out using ball mill to mix；By the cold moudling at room temperature of mixed powder
Bulk is made, pressure is 700~800MPa；The bulk of cold moudling is placed in sinter molding in tube furnace, sinter molding temperature
It it is 850~900 DEG C, soaking time is 20~60 minutes, is protected using flowing argon gas, metal powder is removed by high temperature sintering
Body obtains porous magnetic memorial alloy bulk.
2. the preparation method of porous magnetic memorial alloy according to claim 1, it is characterized in that：The Magnetic memory closes
Gold particle is NiMnGa or NiCoMnIn.
3. the preparation method of porous magnetic memorial alloy according to claim 1 or 2, it is characterized in that：The metal powder
Last particle is spheric granules magnesium powder.
4. the preparation method of porous magnetic memorial alloy according to claim 1 or 2, it is characterized in that：By changing metal
Powder particle content controls porosity.
5. the preparation method of porous magnetic memorial alloy according to claim 3, it is characterized in that：By changing metal powder
Granule content controls porosity.
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| CN201810510957.9A CN108677050A (en) | 2018-05-25 | 2018-05-25 | A kind of preparation method of porous magnetic memorial alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111254310A (en) * | 2020-03-09 | 2020-06-09 | 山东大学 | Preparation method and application of porous nickel |
| CN116083774A (en) * | 2023-04-10 | 2023-05-09 | 成都先进金属材料产业技术研究院股份有限公司 | High magnetic entropy change non-equilibrium state Ni-Co-Mn-In alloy and preparation method and application thereof |
Citations (4)
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| CN101948964A (en) * | 2010-09-16 | 2011-01-19 | 大连理工大学 | Method for preparing biomedical porous titanium and titanium alloy material |
| CN102534282A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Porous Ti-Ni-Mo ternary shape-memory alloy and preparation method thereof |
| CN104357700A (en) * | 2014-11-04 | 2015-02-18 | 东北大学 | Porous titanium and preparing method thereof |
| CN107824784A (en) * | 2017-11-10 | 2018-03-23 | 南昌航空大学 | A kind of preparation method of high-strength light high-damping porous nickel-titanium marmem |
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2018
- 2018-05-25 CN CN201810510957.9A patent/CN108677050A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948964A (en) * | 2010-09-16 | 2011-01-19 | 大连理工大学 | Method for preparing biomedical porous titanium and titanium alloy material |
| CN102534282A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Porous Ti-Ni-Mo ternary shape-memory alloy and preparation method thereof |
| CN104357700A (en) * | 2014-11-04 | 2015-02-18 | 东北大学 | Porous titanium and preparing method thereof |
| CN107824784A (en) * | 2017-11-10 | 2018-03-23 | 南昌航空大学 | A kind of preparation method of high-strength light high-damping porous nickel-titanium marmem |
Non-Patent Citations (3)
| Title |
|---|
| GANG WANG ET AL.: "Study on Powder Metallurgical Preparation of NiCoMnIn Alloy Foam", 《MATERIALS SCIENCE FORUM》 * |
| J.A. MONROE ET AL.: "Magnetic response of porous NiCoMnSn metamagnetic shape", 《SCRIPTA MATERIALIA》 * |
| KOUHEI ITO ET AL.: "Martensitic Transformation in NiCoMnSn Metamagnetic", 《MATERIALS TRANSACTIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111254310A (en) * | 2020-03-09 | 2020-06-09 | 山东大学 | Preparation method and application of porous nickel |
| CN116083774A (en) * | 2023-04-10 | 2023-05-09 | 成都先进金属材料产业技术研究院股份有限公司 | High magnetic entropy change non-equilibrium state Ni-Co-Mn-In alloy and preparation method and application thereof |
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Application publication date: 20181019 |