CN102030521A - Method for preparing M-shaped iron strontium oxide with high coercive force - Google Patents
Method for preparing M-shaped iron strontium oxide with high coercive force Download PDFInfo
- Publication number
- CN102030521A CN102030521A CN 201010524184 CN201010524184A CN102030521A CN 102030521 A CN102030521 A CN 102030521A CN 201010524184 CN201010524184 CN 201010524184 CN 201010524184 A CN201010524184 A CN 201010524184A CN 102030521 A CN102030521 A CN 102030521A
- Authority
- CN
- China
- Prior art keywords
- nitrate
- glycine
- coercive force
- strontium
- precursor powder
- 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.)
- Pending
Links
Images
Landscapes
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a method for preparing an M-shaped iron strontium oxide with a high coercive force, which belongs to the technical field of magnetic materials. Strontium nitrate, ferric nitrate and aluminum nitrate serve as raw materials, and glycine serves as a fuel. The method comprises the following steps of: first dissolving the raw materials and the fuel with distilled water, and performing stirring for 2 to 3 hours; then heating the solution to volatilize the water and generating the precursor powder of SrAlxFe12-xO19 by using the self-propagating combustion of the glycine; and finally pressing the precursor powder into tablets under the pressure of 2 MPa, and sintering the tablets for 2 hours in an air atmosphere at 800 to 1,100 DEG C to generate the SrAlxFe12-xO19 material. The raw materials adopted by the method have low cost; the preparation method ensures simplicity, relatively shorter required time and relatively lower energy consumption; and the prepared SrAlxFe12-xO19 has the high coercive force which can reach more than 15,000 G.
Description
Technical field
The invention belongs to the field of magneticsubstance.The glycine mononitrate preparation method who relates to a kind of high-coercive force M type strontium ferrites is that raw material and glycine are fuel with analytically pure strontium nitrate, iron nitrate, aluminum nitrate, and is synthetic by self-propagating reaction and high temperature sintering technology.
Technical background
The M type strontium ferrites (SrFe of hexagonal structure
12O
19) be a kind of permanent-magnet ferrite, have advantages such as stable performance and oxidation-resistance are strong, therefore, and always at the high-density magneticsubstance, electromagnetic interference, magnetic fluid, fields such as microwave device are used widely.Because the aboundresources of preparation M type strontium ferrites, preparation cost is low, and therefore technology of preparing maturation, simple, carries out the preparation of M type strontium ferrites and the research work of performance, has important use value and economic worth.In recent years, though the preparation of M type strontium ferrite material and the research work of magnetic property obtain some progress, but because its coercive force is far below the permanent magnet material neodymium iron boron that is widely used at present, have a strong impact on its application in the magnetic function device, become the major issue that hinders its application and development.
In recent years, many article reports are arranged, can make SrFe by chemical synthesis process
12O
19Coercive force can reach 6446.9G (Xiaofeng Yang, et al, Journal of Alloys and Compounds, 4752009,312-315); Also there is other scientific research group to pass through La
3+Ion substitution SrFe
L2O
19In Fe
3+Ion, can so that coercive force reach 7000G (T.T.V.Nga, et al, Journal of Alloys andCompounds, 475,2009,55-59); In addition, other researchists are also arranged, can make SrFe by the acid-basicity of adjusting sol gel solution and the method for alternative dopings
12O
19Coercive force reach 5500-6500G (Qi Mixiang etc., State Intellectual Property Office of the People's Republic of China, application number: 200810231633.8; Publication number: CN 101372417).Although people attempt to utilize the whole bag of tricks and technology to improve the coercive force of strontium ferrites, and make progress always, but still, be difficult to, hindered it and used widely and develop with the NdFeB material competition much smaller than the coercitive size of NdFeB material (15000G).
Summary of the invention
The objective of the invention is to adopt Al
3+Adulterated as an alternative method utilizes glycine mononitrate legal system to be equipped with M type SrAl
xFe
12-xO
19(0＜x≤3) solve SrFe
12O
19The problem that the material coercive force is little.
It is that raw material and glycine are fuel that the present invention is characterized in that with analytically pure strontium nitrate, aluminum nitrate, iron nitrate, is the reaction means with the self-propagating reaction of glycine-nitrate process, prepares SrAl
xFe
12-xO
19Precursor powder, then with the precursor powder compressing tablet at air atmosphere, 800～1100 ℃ of following sintering 2 hours can obtain high-coercive force SrAl
xFe
12-xO
19Material.
Implementation process of the present invention is as follows:
A kind of preparation method of high-coercive force M type strontium ferrites, with analytically pure strontium nitrate, iron nitrate and aluminum nitrate is raw material, with the glycine is fuel, consumption is strontium nitrate in molar ratio: iron nitrate: aluminum nitrate=9: 108-9x: 9x, wherein 0＜x≤3, strontium nitrate in molar ratio: glycine=1: 21～64; Preparation process is, with dissolved in distilled water raw material and fuel, stirs 2～3 hours, and heated solution volatilizees water fully then, by the self-propagating combustion of glycine, makes between nitrate and the glycine to react generation SrAl
xFe
12-xO
19Precursor powder; Again the precursor powder is pressed into sheet under 2MPa pressure,, generates SrAl air atmosphere, 800～1100 ℃ of following sintering 2 hours
xFe
12-xO
19Material.
In air atmosphere, 300 ℃ annealing 2 hours down, compacting in flakes again with the precursor powder that generates.The annealed effect is to allow glycine and some organism of not having perfect combustion to fall volatilize away.
Preferred raw material and fuel ratio are strontium nitrates in molar ratio: glycine=1: 32, at this moment the coercive force of resulting sample is higher.
Principal reaction process type of the present invention is:
9Sr(NO
3)
2+(108-9x)Fe(NO
3)
3·9H
2O+9xAl(NO
3)
3·9H
2O+190C
2H
5NO
2→9SrAl
xFe
12-xO
19。
The SrAl that the present invention is prepared
xFe
12-xO
19Material possesses following advantage:
(1) preparation SrAl
xFe
12-xO
19Required raw material strontium nitrate, iron nitrate, aluminum nitrate and fuel glycine all are analytical pure, and cheap.
(2) Zhi Bei technology is fairly simple, and energy consumption is lower.
(3) the required time ratio of whole process of preparation is shorter.
(4) SrAl for preparing
xFe
12-xO
19Coercive force very high, can reach more than the 15000G.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the SrAl that the embodiment of the invention 2 makes
2Fe
10O
19The X-ray diffractogram of precursor powder
Fig. 3 is the SrAl that the embodiment of the invention 2 makes
2Fe
10O
19The X-ray diffractogram.
Fig. 4 is SrAl
2Fe
10O
19Magnetic hysteresis loop figure.
Embodiment
Embodiment 1
With 1.01g strontium nitrate (Sr (NO
3)
2), 22.18g iron nitrate (Fe (NO
3)
39H
2O) and 0.895g aluminum nitrate (Al (NO
3)
39H
2O) put into the beaker of 1000mL as raw material, and add 15.132g glycine (C
2H
5NO
2) act as a fuel, make strontium nitrate: glycine=1: 42 proportioning, dissolved with an amount of distilled water.Beaker is placed on stirred on the ion agitator 2～3 hours, then beaker is placed on the Electric stove sintering and produces out SrAl
0.5Fe
11.5O
19Precursor powder.Precursor powder is collected, and at air atmosphere, annealing is 2 hours in 300 ℃ of pipe type stoves, and glycine and some organism that allowing does not have perfect combustion to fall volatilize away.The grinding tool that with the precursor powder diameter is 5mm is pressed into sheet under the pressure of 2MPa, and in tube furnace air atmosphere, sintering is 2 hours under 1000 ℃ of conditions, obtains SrAl
0.5Fe
11.5O
19Sample, obtaining its coercive force by the VSM test is 7637.5G.
With 1.054g strontium nitrate (Sr (NO
3)
2), 20.119g iron nitrate (Fe (NO
3)
39H
2O) and 3.736g aluminum nitrate (Al (NO
3)
39H
2O) put into the beaker of 1000mL as raw material, and add 11.838g glycine (C
2H
5NO
2) act as a fuel, make strontium nitrate: glycine=1: 32 proportioning, dissolved with an amount of distilled water.Beaker is placed on stirred on the ion agitator 2～3 hours, then beaker is placed on the Electric stove sintering and produces out SrAl
2Fe
10O
19Precursor powder.Precursor powder is collected, and at air atmosphere, annealing is 2 hours in 300 ℃ of pipe type stoves, and glycine and some organism that allowing does not have perfect combustion to fall volatilize away.What Fig. 2 showed is exactly air atmosphere, the X-ray diffractogram of the precursor powder under 300 ℃ of conditions after the annealing, and its main component is Fe
3O
4And SrAl
2O
4The grinding tool that with the precursor powder diameter is 5mm is pressed into sheet under the pressure of 2MPa, and in tube furnace air atmosphere, sintering is 2 hours under 1050 ℃ of conditions, what Fig. 3 showed is exactly 2 hours X-ray diffractogram of 1050 ℃ of following sintering, its main component is SrAl
2Fe
10O
19That Fig. 4 shows is SrAl
2Fe
10O
19The magnetic hysteresis loop figure that sample obtains behind the VSM through test, therefrom we can know and see SrAl
2Fe
10O
19The coercive force of material can reach 12785.9G.
SrAl
2Fe
10O
19EDS power spectrum content as follows:
| Chemical element | Wt％ | At％ |
| OK | 38.16 | 66.88 |
| AlK | 06.70 | 06.96 |
| SrL | 08.40 | 02.69 |
| FeK | 46.74 | 23.47 |
Embodiment 3
With 1.085g strontium nitrate (Sr (NO
3)
2), 18.643g iron nitrate (Fe (NO
3)
39H
2O) and 5.77g aluminum nitrate (Al (NO
3)
39H
2O) put into the beaker of 1000mL as raw material, and add 12.1875g glycine (C
2H
5NO
2) act as a fuel, make strontium nitrate: glycine=1: 32 proportioning, dissolved with an amount of distilled water.Beaker is placed on stirred on the ion agitator 2～3 hours, then beaker is placed on the Electric stove sintering and produces out SrAl
3Fe
gO
19Precursor powder.The grinding tool that with the precursor powder diameter is 5mm is pressed into sheet under the pressure of 2MPa, and in tube furnace air atmosphere, sintering is 2 hours under 1100 ℃ of conditions, obtains SrAl
3Fe
9O
19Sample.Obtaining its coercive force by the VSM test is 16876.9G.
Claims (3)
1. the preparation method of a high-coercive force M type strontium ferrites, with analytically pure strontium nitrate, iron nitrate and aluminum nitrate is raw material, with the glycine is fuel, consumption is strontium nitrate in molar ratio: iron nitrate: aluminum nitrate=9: 108-9x: 9x, wherein 0＜x≤3, strontium nitrate in molar ratio: glycine=1: 21～64; Preparation process is, with dissolved in distilled water raw material and fuel, stirs 2～3 hours, and heated solution volatilizees water fully then, by the self-propagating combustion of glycine, makes between nitrate and the glycine to react generation SrAl
xFe
12-xO
19Precursor powder; Again the precursor powder is pressed into sheet under 2MPa pressure,, generates SrAl air atmosphere, 800～1100 ℃ of following sintering 2 hours
xFe
12-xO
19Material.
2. according to the preparation method of the described a kind of high-coercive force M type strontium ferrites of claim 1, it is characterized in that in air atmosphere, 300 ℃ annealing 2 hours down, compacting in flakes again with the precursor powder that generates.
3. according to the preparation method of claim 1 or 2 described a kind of high-coercive force M type strontium ferritess, it is characterized in that, in molar ratio strontium nitrate: glycine=1: 32.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010524184 CN102030521A (en) | 2010-10-29 | 2010-10-29 | Method for preparing M-shaped iron strontium oxide with high coercive force |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010524184 CN102030521A (en) | 2010-10-29 | 2010-10-29 | Method for preparing M-shaped iron strontium oxide with high coercive force |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102030521A true CN102030521A (en) | 2011-04-27 |
Family
ID=43884042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010524184 Pending CN102030521A (en) | 2010-10-29 | 2010-10-29 | Method for preparing M-shaped iron strontium oxide with high coercive force |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102030521A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106846718A (en) * | 2017-04-07 | 2017-06-13 | 安徽鑫磁源磁业有限公司 | One kind prepares the ferritic warning device of pure M-type strontium |
| WO2020188927A1 (en) * | 2019-03-19 | 2020-09-24 | 富士フイルム株式会社 | Magnetoplumbite-type hexagonal ferrite powder, radio wave absorber, and method for controlling resonant frequency of magnetoplumbite-type hexagonal ferrite powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372417A (en) * | 2008-09-25 | 2009-02-25 | 中国科学院青海盐湖研究所 | High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof |
-
2010
- 2010-10-29 CN CN 201010524184 patent/CN102030521A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372417A (en) * | 2008-09-25 | 2009-02-25 | 中国科学院青海盐湖研究所 | High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《吉林大学硕士学位论文》 20081231 张之胜 纳米磁铅石型锶铁氧体的化学合成与磁性研究 51-53 1-3 , * |
| 《四川大学硕士学位论文》 20031231 肖复勋 添加剂对锶铁氧体永磁磁性能的影响规律及机理探讨 33-34 1-3 , * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106846718A (en) * | 2017-04-07 | 2017-06-13 | 安徽鑫磁源磁业有限公司 | One kind prepares the ferritic warning device of pure M-type strontium |
| WO2020188927A1 (en) * | 2019-03-19 | 2020-09-24 | 富士フイルム株式会社 | Magnetoplumbite-type hexagonal ferrite powder, radio wave absorber, and method for controlling resonant frequency of magnetoplumbite-type hexagonal ferrite powder |
| JPWO2020188927A1 (en) * | 2019-03-19 | 2021-10-28 | 富士フイルム株式会社 | A method for controlling the resonance frequency of a magnetoplumbite-type hexagonal ferrite powder, a radio wave absorber, and a magnetoplumbite-type hexagonal ferrite powder. |
| CN113574021A (en) * | 2019-03-19 | 2021-10-29 | 富士胶片株式会社 | Magnetoplumbite-type hexagonal ferrite powder, radio wave absorber, and method for controlling resonance frequency of magnetoplumbite-type hexagonal ferrite powder |
| JP7179959B2 (en) | 2019-03-19 | 2022-11-29 | 富士フイルム株式会社 | Magnetoplumbite-type hexagonal ferrite powder, radio wave absorber, and method for controlling resonance frequency of magnetoplumbite-type hexagonal ferrite powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103964828B (en) | A kind of high-performance permanent magnetic ferrite material and preparation method thereof | |
| WO2016141625A1 (en) | Method for preparing neodymium-iron-boron magnet by utilizing waste material and neodymium-iron-boron magnet | |
| CN103187133B (en) | A kind of RE permanent magnetic alloy and Magnetic Phase composite preparation process thereof | |
| CN109192495B (en) | Preparation method of regenerative sintered neodymium-iron-boron permanent magnet | |
| CN103834863B (en) | The method of Nd-Fe-Bo permanent magnet material is manufactured with common association mishmetal | |
| CN102757235B (en) | Permanent magnetic strontium-ferrite material powder and preparation method thereof | |
| CN103449808B (en) | Preparation method of biphase composite hard magnetic ferrite nano-powder with exchange coupling | |
| CN104211388B (en) | One is suitable for low sintering M-type strontium ferrite SrFe 12o 19preparation method | |
| CN104529424A (en) | Composite permagnetferrite with functions of two-phase exchange coupling and keeping high coercive force | |
| CN105601265A (en) | M-type strontium ferrite magnetic material and method for preparing same | |
| CN103413644A (en) | Method for preparing samarium cobalt magnetic powder | |
| CN102360909B (en) | Preparation method for neodymium iron boron magnet | |
| CN101229931B (en) | Method for preparing nano Fe3O4 | |
| CN102030521A (en) | Method for preparing M-shaped iron strontium oxide with high coercive force | |
| CN105016395A (en) | Nano ferrite material, and preparation method thereof | |
| CN102129906B (en) | Permanent ferrite material additive and preparation method and application thereof | |
| CN102924069A (en) | Hexagonal crystal M+W mixed type sintered permanent magnetic ferrite magnet and preparation method thereof | |
| CN109206131A (en) | A kind of rear-earth-doped M-type strontium ferrite magnetic material and preparation method thereof | |
| CN103317146B (en) | Hydro-thermal method prepares the method for NdFeB magnetic powder | |
| CN104404255A (en) | Simplified method for pretreatment-acid leaching of neodymium iron boron waste material | |
| CN102839301A (en) | Rare earth coblat-based alloy, alloy powder and manufacturing method of alloy and alloy powder | |
| CN105439208A (en) | Method for preparing permanent magnet strontium ferrite by utilizing iron oxide red | |
| CN102898129B (en) | La-Zn co-doping permanent magnetic strontium ferrite material powder and preparation method thereof | |
| US20110031432A1 (en) | Mechanical improvement of rare earth permanent magnets | |
| Mansouri et al. | Waste of batteries management: Synthesis of magnetocaloric manganite compound from the REEs mixture generated during hydrometallurgical processing of NiMH batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110427 |