CN102392113A - Device and process for carrying out heat treatment on nanometer composite permanent-magnetic materials - Google Patents
Device and process for carrying out heat treatment on nanometer composite permanent-magnetic materials Download PDFInfo
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- CN102392113A CN102392113A CN2011103563813A CN201110356381A CN102392113A CN 102392113 A CN102392113 A CN 102392113A CN 2011103563813 A CN2011103563813 A CN 2011103563813A CN 201110356381 A CN201110356381 A CN 201110356381A CN 102392113 A CN102392113 A CN 102392113A
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Abstract
The invention discloses device and process for carrying out heat treatment on nanometer composite permanent-magnetic materials. The device comprises a sealed cavity, a heating body, vacuum pumping equipment, temperature control equipment, a cooling water pipe and water supply equipment, wherein the heating body takes the shape of square which is opened rightwards; a wheel track is arranged below the heating body; the vacuum pumping equipment is communicated with the sealed cavity through a rubber pipe; the temperature control equipment is connected with the heating body through a conductor; the cooling water pipe is connected with the water supply equipment through a plastic pipe; a valve is arranged on the plastic pipe; and a water injection nozzle is arranged at the lower part of the cooling water pipe. By using the heat treatment device, the aim of carrying out rapid warming and rapid cooling on nanometer composite permanent-magnetic materials can be realized, so that nanometer crystallization occurs on amorphous structures of the materials, the microstructures of the nanometer materials are effectively improved and the magnetic performance of the nanometer composite permanent-magnetic materials are increased. Furthermore, the heat treatment device is simple in structure and the heat treatment process is convenient for operation.
Description
Technical field
The present invention relates to a kind of device that nano composite permanent magnetic material is heat-treated and uses this thermal treatment unit to the thermal treatment process that nano composite permanent magnetic material carries out, and belongs to the material heat treatment technical field.
Background technology
Nano composite permanent magnetic material provides high saturation magnetization mutually by soft magnetism; Hard Magnetic provides high magnetocrystalline anisotropy field mutually; Two are composited in nanoscale; Have low content of rare earth, high remanent magnetism, high relatively coercive force and high good characteristics such as theoretical magnetic energy product, therefore become the focus of domestic and international research.Yet expecting the ideal microstructure, generally all is earlier with the material melting ingot casting of certain alloying constituent, in quick quenching furnace, prepares amorphous thin ribbon, after amorphous structure annealing thermal treatment, generates nanostructure and realizes the fine magnetic property of material.The annealing device that uses at present generally all is that vacuum furnace chamber and heating system are structure as a whole; When material is heat-treated; All be progressively to be increased to hot stage from low thermophase, amorphous structure very easily produces the grain growth phenomenon in such treating processes, can not realize material nanoization.Simultaneously, traditional annealing device does not possess good cooling system, generally all is furnace cooling, is unfavorable for producing nano-crystallization equally.For this reason, how to provide a kind of to nano composite permanent magnetic material be rapidly heated, fast refrigerative thermal treatment unit and thermal treatment process, become the technical problem that industry needs to be resolved hurrily.
Summary of the invention
To existing in prior technology the problems referred to above and demand; The purpose of this invention is to provide a kind of device and technology that nano composite permanent magnetic material is heat-treated; With realization nano composite permanent magnetic material is rapidly heated, cools off fast; Make the amorphous structure of material produce nano-crystallization, thereby effectively improve the microstructure of nano material, improve the purpose of magnetism of material ability.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of device that nano composite permanent magnetic material is heat-treated comprises: enclosed housing, heating member, vaccum-pumping equipment, temperature control device, water-cooled tube and water equipment; Described heating member is the Contraband font, and wheel track thereunder is housed, and moves heating member through wheel track, realizes that heating member shrouds enclosed housing or moves apart enclosed housing; Described vaccum-pumping equipment is connected with enclosed housing through rubber tubing; Described temperature control device is connected with heating member through lead; Described water-cooled tube is connected with water equipment through plastic conduit; Described plastic conduit is provided with valve; Described water-cooled tube bottom is provided with water jet.
Described enclosed housing preferably ceramic pipe or silica tube.
Described enclosed housing preferably fixes on the ground with level, cantilevered fashion.
A kind ofly use above-mentioned thermal treatment unit, comprise the steps: the nano composite permanent magnetic material heat-treating process
A) amorphous ribbon of nano composite permanent magnetic material is put into the enclosed housing of said thermal treatment unit;
B) open vaccum-pumping equipment enclosed housing is vacuumized processing;
C) start temperature control device, set heating member temperature and TRT, heating member is implemented warming temperature;
When d) body to be heated reached the temperature of setting and vacuum tightness that enclosed housing reaches setting, the wheel track through the heating member bottom moves heating member made it shroud enclosed housing, and the amorphous ribbon of the intravital nano composite permanent magnetic material of annular seal space is implemented rapid heating and insulation;
E) soaking time finishes, and the wheel track bottom heating member moves heating member makes it move apart enclosed housing;
F) valve of opening on the water equipment is implemented rapid water-cooled operation to enclosed housing.
The set(ting)value of the heating member temperature in the step c) is recommended as 680～730 ℃.
The heating member TRT in the step c) recommends to be made as 20～50 minutes.
Vacuum tightness described in the step d) recommends≤3 * 10
-3Pa.
Soaking time in the step e) is recommended as 5～15 minutes.
The present invention adopts heating member and the separable design feature of enclosed housing; Make described thermal treatment unit realized to nano composite permanent magnetic material be rapidly heated, quick cooling purpose; Thereby make the amorphous structure of material can produce nano-crystallization; Effectively improve the microstructure of nano material, reached the beneficial effect that improves the magnetic property of nano composite permanent magnetic material; And described thermal treatment unit has simple in structurely, and that described thermal treatment process has is simple to operate, advantage easily, is fit to wide popularization and application.
Description of drawings
Fig. 1 is the structural representation of the thermal treatment unit described in the embodiment.
Fig. 2 is the map of the transmission electron microscope photo before and after the amorphous ribbon of the nano composite permanent magnetic material described in the embodiment 1 is heat-treated, wherein: the pattern photo before a representes to handle, the pattern photo after b representes to handle.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Embodiment 1
As shown in Figure 1, a kind of device that nano composite permanent magnetic material is heat-treated provided by the invention comprises: enclosed housing 1, heating member 2, vaccum-pumping equipment 3, temperature control device 4, water-cooled tube 5 and water equipment 6; Described heating member 2 is the Contraband font, and wheel track 21 thereunder is housed, and moves heating member 2 through wheel track 21, can realize that heating member 2 shrouds enclosed housing 1 or moves apart enclosed housing 1; Described vaccum-pumping equipment 3 is connected with enclosed housing 1 through rubber tubing 7; Described temperature control device 4 is connected with heating member 2 through lead 8; Described water-cooled tube 5 is connected with water equipment 6 through plastic conduit 9; Described plastic conduit 9 is provided with valve 10; The bottom of described water-cooled tube 5 is provided with water jet 51.
Described enclosed housing 1 preferably ceramic pipe or silica tube preferably fixes on the ground with level, cantilevered fashion.
Use above-mentioned thermal treatment unit following: the amorphous ribbon of the nano composite permanent magnetic material for preparing to be put into enclosed housing 1, open 3 pairs of enclosed housings 1 of vaccum-pumping equipment and vacuumize processing to the nano composite permanent magnetic material heat-treating process; Simultaneously, start temperature control device 4, the temperature of setting heating member 2 is 710 ℃, and the TRT is 30min, and heating member 2 is implemented warming temperature; The vacuum tightness that temperature reaches in 710 ℃ of set(ting)values and the enclosed housing 1 in the body 2 to be heated reaches 2 * 10
-3During Pa, move heating member 2,, the amorphous ribbon of the intravital nano composite permanent magnetic material of annular seal space is implemented rapid heating and is incubated 10min to realize that heating member 2 shrouds enclosed housing 1 through wheel track 21; Treat that soaking time finishes, the wheel track 21 bottom heating member moves heating member 2 makes it move apart enclosed housing 1; Open the valve 10 on the plastic conduit 9 between water equipment 6 and the water-cooled tube 5, implement rapid water-cooled operation through the 51 pairs of enclosed housings of water jet 1 that are located at water-cooled tube 5 bottoms.
Fig. 2 is the map of the transmission electron microscope photo before and after the amorphous ribbon of the nano composite permanent magnetic material described in the present embodiment is heat-treated, wherein: the pattern photo before a representes to handle, the pattern photo after b representes to handle; Visible by Fig. 2: the amorphous ribbon of nano composite permanent magnetic material is before heat-treating, and the inside particle of material is the state of short range order, is non-crystal structure completely; But after above-mentioned thermal treatment, amorphous structure crystallization is a nanostructure, and grain-size is about about 30nm.
Adopt the maximum magnetic energy product of vibrating sample magnetometer test material, test data is 120kJ/m
3, the visible request for utilization that can satisfy permanent magnet material.
Use the thermal treatment unit described in the embodiment 1 following: the amorphous ribbon of the nano composite permanent magnetic material for preparing to be put into enclosed housing 1, open 3 pairs of enclosed housings 1 of vaccum-pumping equipment and vacuumize processing to the nano composite permanent magnetic material heat-treating process; Simultaneously, start temperature control device 4, the temperature of setting heating member 2 is 680 ℃, and the TRT is 50min, and heating member 2 is implemented warming temperature; The vacuum tightness that temperature reaches in 680 ℃ of set(ting)values and the enclosed housing 1 in the body 2 to be heated reaches 3 * 10
-3During Pa, move heating member 2,, the amorphous ribbon of the intravital nano composite permanent magnetic material of annular seal space is implemented rapid heating and is incubated 15min to realize that heating member 2 shrouds enclosed housing 1 through wheel track 21; Treat that soaking time finishes, the wheel track 21 bottom heating member moves heating member 2 makes it move apart enclosed housing 1; Open the valve 10 on the plastic conduit 9 between water equipment 6 and the water-cooled tube 5, implement rapid water-cooled operation through the 51 pairs of enclosed housings of water jet 1 that are located at water-cooled tube 5 bottoms.
After above-mentioned thermal treatment, the amorphous structure of nano composite permanent magnetic material has produced nano-crystallization, and grain-size is about 40nm.
Adopt the maximum magnetic energy product of vibrating sample magnetometer test material, test data is 108kJ/m
3, the visible request for utilization that can satisfy permanent magnet material.
Use the thermal treatment unit described in the embodiment 1 following: the amorphous ribbon of the nano composite permanent magnetic material for preparing to be put into enclosed housing 1, open 3 pairs of enclosed housings 1 of vaccum-pumping equipment and vacuumize processing to the nano composite permanent magnetic material heat-treating process; Simultaneously, start temperature control device 4, the temperature of setting heating member 2 is 730 ℃, and the TRT is 20min, and heating member 2 is implemented warming temperature; The vacuum tightness that temperature reaches in 730 ℃ of set(ting)values and the enclosed housing 1 in the body 2 to be heated reaches 1 * 10
-3During Pa, move heating member 2,, the amorphous ribbon of the intravital nano composite permanent magnetic material of annular seal space is implemented rapid heating and is incubated 5min to realize that heating member 2 shrouds enclosed housing 1 through wheel track 21; Treat that soaking time finishes, the wheel track 21 bottom heating member moves heating member 2 makes it move apart enclosed housing 1; Open the valve 10 on the plastic conduit 9 between water equipment 6 and the water-cooled tube 5, implement rapid water-cooled operation through the 51 pairs of enclosed housings of water jet 1 that are located at water-cooled tube 5 bottoms.
After above-mentioned thermal treatment, the amorphous structure of nano composite permanent magnetic material has produced nano-crystallization, and grain-size is about 35nm.
Adopt the maximum magnetic energy product of vibrating sample magnetometer test material, test data is 115kJ/m
3, the visible request for utilization that can satisfy permanent magnet material.
Visible in sum: as to adopt heat treatment technics of the present invention, can make the amorphous structure of nano composite permanent magnetic material produce nano-crystallization, effectively improve the microstructure of nano material, improve the magnetic property of nano composite permanent magnetic material.
Should be noted that at last: above embodiment only is used for the present invention is described further; Can not be interpreted as the restriction to protection domain of the present invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (8)
1. the device that nano composite permanent magnetic material is heat-treated is characterized in that, comprising: enclosed housing, heating member, vaccum-pumping equipment, temperature control device, water-cooled tube and water equipment; Described heating member is the Contraband font, and wheel track thereunder is housed, and moves heating member through wheel track, realizes that heating member shrouds enclosed housing or moves apart enclosed housing; Described vaccum-pumping equipment is connected with enclosed housing through rubber tubing; Described temperature control device is connected with heating member through lead; Described water-cooled tube is connected with water equipment through plastic conduit; Described plastic conduit is provided with valve; Described water-cooled tube bottom is provided with water jet.
2. device according to claim 1 is characterized in that: described enclosed housing is vitrified pipe or silica tube.
3. device according to claim 1 is characterized in that: described enclosed housing fixes on the ground with level, cantilevered fashion.
4. an application rights requires 1 described device to the nano composite permanent magnetic material heat-treating process, it is characterized in that, comprises the steps:
A) amorphous ribbon of nano composite permanent magnetic material is put into the enclosed housing of said thermal treatment unit;
B) open vaccum-pumping equipment enclosed housing is vacuumized processing;
C) start temperature control device, set heating member temperature and TRT, heating member is implemented warming temperature;
When d) body to be heated reached the temperature of setting and vacuum tightness that enclosed housing reaches setting, the wheel track through the heating member bottom moves heating member made it shroud enclosed housing, and the amorphous ribbon of the intravital nano composite permanent magnetic material of annular seal space is implemented rapid heating and insulation;
E) soaking time finishes, and the wheel track bottom heating member moves heating member makes it move apart enclosed housing;
F) valve of opening on the water equipment is implemented rapid water-cooled operation to enclosed housing.
5. technology according to claim 4 is characterized in that: the set(ting)value of the heating member temperature in the step c) is 680～730 ℃.
6. technology according to claim 4 is characterized in that: the heating member TRT in the step c) was made as 20～50 minutes.
7. technology according to claim 4 is characterized in that: the vacuum tightness described in the step d)≤3 * 10
-3Pa.
8. technology according to claim 4 is characterized in that: the soaking time in the step e) is 5～15 minutes.
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| CN2011103563813A CN102392113A (en) | 2011-11-11 | 2011-11-11 | Device and process for carrying out heat treatment on nanometer composite permanent-magnetic materials |
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| CN2011103563813A CN102392113A (en) | 2011-11-11 | 2011-11-11 | Device and process for carrying out heat treatment on nanometer composite permanent-magnetic materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104164636A (en) * | 2014-06-30 | 2014-11-26 | 中磁科技股份有限公司 | Thermal processing method of neodymium-iron-boron casting strip and thermal processing device |
| CN104962706A (en) * | 2015-07-07 | 2015-10-07 | 长兴县大云电炉制造有限公司 | Electromagnetic induction furnace for carrying out heat treatment on amorphous and nanocrystalline materials |
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| CN201148450Y (en) * | 2008-01-24 | 2008-11-12 | 扬州诚德钢管有限公司 | Steel tube quenching equipment |
| CN201212046Y (en) * | 2008-06-27 | 2009-03-25 | 中国科学院沈阳科学仪器研制中心有限公司 | Vacuum annealing furnace |
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| CN201148450Y (en) * | 2008-01-24 | 2008-11-12 | 扬州诚德钢管有限公司 | Steel tube quenching equipment |
| CN201212046Y (en) * | 2008-06-27 | 2009-03-25 | 中国科学院沈阳科学仪器研制中心有限公司 | Vacuum annealing furnace |
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| 《中国优秀博硕士学位论文全文数据库（博士）工程科技Ⅰ辑》 20060915 王晨 纳米复合Nd2Fe14B/alpha-Fe永磁材料微结构和磁性能研究 26、27 1-8 , * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104164636A (en) * | 2014-06-30 | 2014-11-26 | 中磁科技股份有限公司 | Thermal processing method of neodymium-iron-boron casting strip and thermal processing device |
| CN104962706A (en) * | 2015-07-07 | 2015-10-07 | 长兴县大云电炉制造有限公司 | Electromagnetic induction furnace for carrying out heat treatment on amorphous and nanocrystalline materials |
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Application publication date: 20120328 |