CN1100472A - Pulse current treatment for producing iron-base nano-meter crystal material - Google Patents
Pulse current treatment for producing iron-base nano-meter crystal material Download PDFInfo
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- CN1100472A CN1100472A CN 93115804 CN93115804A CN1100472A CN 1100472 A CN1100472 A CN 1100472A CN 93115804 CN93115804 CN 93115804 CN 93115804 A CN93115804 A CN 93115804A CN 1100472 A CN1100472 A CN 1100472A
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Abstract
Amorphous alloy belt or wire is electrical pulse treated by means of connection to the output terminal of pulse current generator via excellent conductive fixture. Pulse freq., current density, pulse width and treatment period are regulated based on the different amorphous material and its composition, and the specimen temp. is measured with thermometric instrument, such as a platinum membrane resistance temp. sensor. The produced nanometer crystal material of different sizes may be widely used in catalyst, optical filter material, photoabsorption magnetic medium and other new material.
Description
The present invention relates to the preparation method of nanocrystalline solids material, particularly a kind of nano-crystalline magnetic material.
At present, along with science and technology development, nanocrystalline material will become the important materials of high-technology field from now on, and it has many high-performances, and application prospect will be more and more widely.Lattice Lay top grade people reported the novel material of nanocrystalline (1-50nm) at first in 1986, its preparation method is the condensation of gas method, was published in 43 pages (1986) of " Japanese metal association journal (supplementary issue) " 27 volumes by Bai Lingeer, Ge Laite.People such as Wang Jing Tang of Metal Inst., Chinese Academy of Sciences proposed with crystallization process from the noncrystal preparation of nano crystal that changes in 1991, be published in 522 pages (1991) of " Applied Physics " magazine 69 volumes, this author in 1993 has reported again with crystallization process and has prepared the nanocrystalline of ferrous alloy that crystal grain diameter is that 45nm is published in " material science and technology " 9 volume 142 pages of 2 phases (1993).The nanocrystalline material of above-mentioned prior art for preparing all needs special equipment, and technological process is complicated.As the condensation of gas method, whole process of preparation need be carried out in that ultrahigh vacuum(HHV) is indoor, has both needed to make the heating unit of metal atomization, needs to make the cryogenic unit of its condensation again, and the nanocrystalline particulate compacting that will obtain with ultra-high voltage forms laminar nanocrystalline then.It is nanocrystalline method that the annealed thermal treatment of amorphous ribbon makes it crystallization, i.e. crystallization method is though its preparation process is simplified to some extent, but thermal treatment temp is higher, strict to temperature and temperature rate, and need a cover insulation, the temperature control system of heating and cooling, vacuum system.Thereby this technology also has great difficulty, has influenced preparation, development and application to nanocrystalline material.
In view of the deficiency that the nanocrystalline technology of existing preparation exists, it is simple to the objective of the invention is to propose a kind of specific installation, technological process of not needing, and prepares the method for iron based nano crystal material.
For achieving the above object, the present invention realizes by following steps.With amorphous alloy band or silk, place on the anchor clamps earlier, be connected on two electrodes of impulse current generator output terminal, again thermistor is attached on the exemplar surface, according to the difference of amorphous material and composition, adjusts pulsed current then, frequency 10-30HZ, pulse current density Jmax 1.0 * 10
3～5.0 * 10
3A/mm
2, pulse width 20～80/us in 10～100 minutes treatment times, with the steady temperature of temperature instrumentation measurement during burst process, can prepare nanocrystalline material.
The present invention can also realize by following measure.Pulsed current is adjusted into frequency 15-25HZ, current density, J max 1.5 * 10
3～3 * 10
3A/mm
2, pulse width 30-60/us, treatment time 20-80 minute, hot resistance adopted platinum film, and common constant temperature rise is 200-250 ℃ for the Fe-Si-B alloy.
Principle of work of the present invention is to utilize the pulsation of current effect of electricimpulse and rapid heating and cooling effect thereof to make non-crystalline state under temperature (Fe-Si-B is about the 550 °) condition far below general crystallization crystallization take place, by the adjusting electric pulse parameter, and make the nanocrystalline of various grain sizes.Because the singularity of the nano microcrystalline structure of matter makes its structure dependent performance than crystal, the sizable variation of noncrystal generation, causes it having a wide range of applications aspect materials such as catalysis, optical filtering, photoabsorption, magneticmedium.
The present invention compared with prior art has following advantage:
1. do not need vacuum system and protective atmosphere, preparation process is simple and easy to do.
2. can access partially-crystallized and all crystallization and different nanocrystalline granularity materials, to satisfy different purposes needs.
Below in conjunction with embodiment the present invention is further specified.
Embodiment one
Adopt Fe
78Si
9B
13Non-crystaline amorphous metal carries out burst process.Earlier amorphous alloy is cleaned, measure resistance value then exactly, for ease of regulating current density.Again exemplar is placed on the chuck of anchor clamps, anchor clamps must clamp, so that maintenance good electrical conductivity, in order to avoid the generation spark discharge, with the platinum film thermistor by spring application on exemplar, so that the steady temperature of exemplar during measuring electricimpulse and handling, make pulse current generator power supply again, the recording processing time, pending finishing takes off exemplar and carries out other commercial measurement.The adjustment power frequency is 20HZ, current density 1.8 * 10
3A/mm
2, pulse width 40/us, in 65 minutes treatment times, the exemplar steady temperature is 200 ℃.
Embodiment two
Operation steps is with embodiment one, but power frequency is 15HZ, current density 3.0 * 10
3A/mm
2, pulse width 20/us, treatment time 100 minutes, 220 ℃ of exemplar surface steady temperatures.
Embodiment three
Operation steps is with embodiment one, but power frequency is 30HZ, current density 5 * 10
3A/mm
2, width 60/us, 10 minutes treatment times, 250 ℃ of exemplar surface steady temperatures.
Claims (4)
1, a kind of method of pulse current treatment for producing iron-base nano-meter crystal material, it is characterized in that: earlier with amorphous alloy band or silk, place on the anchor clamps, be connected on two electrodes of impulse current generator output terminal, thermistor is attached on the exemplar surface again, adjust pulsed current then, frequency 10-30HZ, pulse current density J
Ax1.0 * 10
3～5.0 * 10
3A/mm
2, pulse width 20～80 μ s, 10～100 minutes treatment times,, can prepare nanocrystalline material with the steady temperature of temperature instrumentation measurement during burst process.
2, the method for preparing nanocrystalline material according to claim 1, it is characterized in that: earlier with amorphous alloy band or silk, place on the anchor clamps, be connected on two electrodes of impulse current generator output terminal, thermistor is attached on the exemplar surface again, adjust pulsed current then, frequency 15-25HZ, current density, J max 1.5 * 10
3-3 * 10
3A/mm
2, pulse width 30-60/us, treatment time 20-80 minute, and with temperature instrumentation measurement steady temperature.
3, the method for preparing nanocrystalline material according to claim 1 and 2, it is characterized in that: said thermistor is to use platinum film.
4, the method for preparing nanocrystalline material according to claim 3 is characterized in that: it is 200-250 ℃ that exemplar records steady temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115804 CN1032594C (en) | 1993-09-14 | 1993-09-14 | Pulse current treatment for producing iron-base nano-meter crystal material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115804 CN1032594C (en) | 1993-09-14 | 1993-09-14 | Pulse current treatment for producing iron-base nano-meter crystal material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1100472A true CN1100472A (en) | 1995-03-22 |
| CN1032594C CN1032594C (en) | 1996-08-21 |
Family
ID=4991339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93115804 Expired - Fee Related CN1032594C (en) | 1993-09-14 | 1993-09-14 | Pulse current treatment for producing iron-base nano-meter crystal material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1032594C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322160C (en) * | 2004-08-30 | 2007-06-20 | 清华大学 | Process for preparing block nano crystal/non-crystal alloy |
| CN101705340B (en) * | 2009-11-03 | 2011-07-20 | 上海大学 | Method and device for thermally treating pulse current |
| CN105216136A (en) * | 2014-06-27 | 2016-01-06 | 卡米尔工矿业协助公司 | Pulse power recirculation contains the apparatus and method of the composite of reinforce and matrix |
| CN113444871A (en) * | 2021-07-21 | 2021-09-28 | 山西阳煤化工机械（集团）有限公司 | Method for regulating and controlling strengthening and toughening of ferritic stainless steel based on high-frequency pulse current |
-
1993
- 1993-09-14 CN CN 93115804 patent/CN1032594C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322160C (en) * | 2004-08-30 | 2007-06-20 | 清华大学 | Process for preparing block nano crystal/non-crystal alloy |
| CN101705340B (en) * | 2009-11-03 | 2011-07-20 | 上海大学 | Method and device for thermally treating pulse current |
| CN105216136A (en) * | 2014-06-27 | 2016-01-06 | 卡米尔工矿业协助公司 | Pulse power recirculation contains the apparatus and method of the composite of reinforce and matrix |
| CN105216136B (en) * | 2014-06-27 | 2019-12-03 | 卡米尔工矿业协助公司 | The device and method of composite material of the pulse power recycling containing reinforcer and matrix |
| CN113444871A (en) * | 2021-07-21 | 2021-09-28 | 山西阳煤化工机械（集团）有限公司 | Method for regulating and controlling strengthening and toughening of ferritic stainless steel based on high-frequency pulse current |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1032594C (en) | 1996-08-21 |
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