CN101913854A - Preparation method of nanometer strontium ferrite magnetic powder - Google Patents
Preparation method of nanometer strontium ferrite magnetic powder Download PDFInfo
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- CN101913854A CN101913854A CN 201010255857 CN201010255857A CN101913854A CN 101913854 A CN101913854 A CN 101913854A CN 201010255857 CN201010255857 CN 201010255857 CN 201010255857 A CN201010255857 A CN 201010255857A CN 101913854 A CN101913854 A CN 101913854A
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Abstract
The invention relates to the production of magnetic materials, in particular to a preparation method of nanometer strontium ferrite magnetic powder (SrFe12O19), comprising the following specific steps of: weighting strontium carbonate and ferric nitrate crystal according to the mole ratio of 1:12 of Sr and Fe, solving the strontium carbonate and the ferric nitrate crystal by nitric acid and deionized water, adding tartaric acid and polyethylene glycol after evenly mixing, and regulating the pH value to be 7 by using ammonia water; and heating the obtained mixed liquid to be sol-gel, drying the sol-gel, and carrying out the sectional roasting on the dried sol-gel at 860-1,100 DEG C to prepare powdery magnetic nanometer strontium ferrite. Due to the synergistic effect of the polyethylene glycol, the tartaric acid is used for the first time as a main complexing agent to prepare strontium ferrite so that a precursor directionally grows up, the anisotropy is increased and the saturation magnetization strength Ms is improved. The test shows that the crystallite dimension is 20-45nm, the saturation magnetization strength Ms is 78.4emu/g, and the intrinsic coercivity is 3163.3G. The excellent performance of the magnetic powder is suitable for automobile motor magnets and magnetic recording media materials.
Description
Technical field
The present invention relates to the manufacturing of magneticsubstance, particularly nanometer strontium ferrite magnetic powder (SrFe
12O
19) the preparation method.
Background technology
Nanometer strontium ferrite magnetic powder (SrFe
12O
19) have higher coercive force and saturation magnetization, because of having stable chemical properties, it is widely used in permanent magnet material, microwave absorbing material and high-density perpendicular magnetic recording dielectric material.Sol-gel method is the common method of preparation nano-magnetic strontium ferrites, and it has, and raw material mixes, sintering temperature is low, resultant forms and substitutional ion is controlled easily, particle diameter is little, narrow particle size distribution and characteristics such as have excellent magnetic characteristics.Strontium ferrites is number two at the consumption of Strontium carbonate powder industry, is widely used in industries such as motor, computer, the network information, communication, aerospace, automobile and household electrical appliance.From the eighties in 20th century, the research of strontium ferrites has become the focus of domestic and international research.At present the research emphasis of strontium ferrites towards novel process more, realize that doping diversification, filming and low-dimensional direction develop, purpose is to improve the comprehensive magnetic property of strontium ferrites, thereby obtains to have the ferrite of excellent intrinsic magnetic properties.Common high performance permanent-magnet ferrite must satisfy following two key indexs: 1. have high saturation and magnetic intensity Ms and 2. have significant magnetocrystalline anisotropy K.Usually adopt the citric acid sol-gel process to prepare silver-colored ferrite powder, with polyvinyl alcohol as dispersion agent, thereby strengthen the complex ability of citric acid and metal ion.People such as Huang Ying are presoma preparation non-stoichiometric colloidal sol with strontium nitrate and iron nitrate inorganic salt in " preparing nanometer strontium ferrite magnetic powder with sol-gel method " literary composition, adopt citric acid-gel method to prepare nano-strontium ferrite, maximum value Hc=454.16kA/m appears in its coercive force, and specific saturation magnetization is 55.91A.m
2/ kg.The product magnetic property that method for preparing goes out is lower.In the sol-gel method, do not see that with tartrate be the report that main complexing agent prepares nanometer strontium ferrite magnetic powder at present.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method of nanometer strontium ferrite magnetic powder, it is main complexing agent that present method adopts tartrate, polyoxyethylene glycol is a complexing-aid agent, make the presoma oriented growth, anisotropy increases, thereby nanometer strontium ferrite magnetic powder HCJ and saturation magnetization are significantly improved, and this preparation method is pollution-free to burner hearth.
For achieving the above object, technical scheme of the present invention is:
The preparation method of nanometer strontium ferrite magnetic powder may further comprise the steps:
The a batching: by Sr and Fe mol ratio is 1: 12, and taking by weighing Strontium carbonate powder and iron nitrate crystal is Fe (NO
3)
39H
2O with nitric acid and deionized water dissolving, mixes the back and adds tartrate and polyoxyethylene glycol, and regulating pH with ammoniacal liquor is 7, makes mixed solution; Used tartaric mole number is equivalent to Strontium carbonate powder and iron nitrate crystal mole number sum 1 times;
The preparation of b xerogel: step a gained mixed solution is heated into colloidal sol, further be heated into gel, and drying makes xerogel;
The preparation of c nanometer strontium ferrite magnetic powder: is to carry out the segmentation roasting under 860 ℃～1100 ℃ conditions with step b gained xerogel in top temperature, generates the nano-strontium ferrite magnetic powder, and its molecular formula is SrFe
12O
19
Further, polyoxyethylene glycol described in the step a is a polyoxyethylene glycol-2000, and its concentration in mixed solution is 1.0～1.5g/100m1;
Further, step b is to be heated into colloidal sol under 50 ℃ of conditions with described mixed solution in temperature, is to be heated into gel under 70～80 ℃ of conditions in temperature;
Further, step c is to carry out the segmentation roasting under 860 ℃ of conditions with xerogel in top temperature, and being specially the fs is 36～250 ℃, 5 ℃/min of temperature rise rate; Subordinate phase is 250～500 ℃, 7 ℃/min of temperature rise rate; Phase III is 500～860 ℃, 10 ℃/min of temperature rise rate, again in 860 ℃ of constant temperature 2 hours, nanometer strontium ferrite magnetic powder, its molecular formula is SrFe
12O
19
Further, step c is to carry out the segmentation roasting under 1100 ℃ of conditions with xerogel in top temperature, and be specially: the fs is 23～320 ℃, 5 ℃/min of temperature rise rate; Subordinate phase is 320～650 ℃, 7 ℃/min of temperature rise rate; Phase III is 650～1100 ℃, 10 ℃/min of temperature rise rate, again in 1100 ℃ of constant temperature 2 hours, nanometer strontium ferrite magnetic powder, its molecular formula is SrFe
12O
19
Beneficial effect of the present invention is: present method cost of material is low, can strict control stoichiometric ratio, and technology is simple, and reaction time is short, and the product particle diameter is little, be evenly distributed, and is pollution-free to burner hearth, enlarged the demand area of complexing agent simultaneously; The nanometer strontium ferrite magnetic powder HCJ and the saturation magnetization of present method preparation are significantly improved, and after tested, grain-size is 20～45nm, and saturation magnetization Ms is 78.4emu/g, and HCJ is 3163.3G.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, wherein:
It is the infrared spectrum of nanometer strontium ferrite magnetic powder after the segmentation roasting under 860 ℃ of conditions that Fig. 1 (a) and (b) are respectively the infrared spectrum of xerogel and top temperature;
Fig. 2 is magnetic X-ray diffraction (XRD) spectrogram of the nano-strontium ferrite after the segmentation roasting under 860 ℃ of conditions for top temperature;
Fig. 3 is the magnetic hysteresis loop of the nanometer strontium ferrite magnetic powder after the segmentation roasting under 860 ℃ of conditions for top temperature;
Fig. 4 is the X-ray diffraction spectrogram of the nanometer strontium ferrite magnetic powder after the segmentation roasting under 1100 ℃ of conditions for top temperature;
Fig. 5 is the magnetic hysteresis loop of the nanometer strontium ferrite magnetic powder after the segmentation roasting under 1100 ℃ of conditions for top temperature.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
The preparation of embodiment 1 nanometer strontium ferrite magnetic powder
Taking by weighing 20.1420g iron nitrate crystal is Fe (NO
3)
39H
2O is dissolved in the 50ml deionized water, takes by weighing 0.6169g Strontium carbonate powder (SrCO
3) drip a small amount of salpeter solution until dissolving fully, with Strontium carbonate powder lysate and iron nitrate solution mixing and stirring.Sr and Fe mol ratio are 1: 12 in the above-mentioned mixed solution.8.1327g tartrate is dissolved in the mixed solution, adds 0.5601g polyoxyethylene glycol-2000 stirring and dissolving again after treating to dissolve fully.PH value with the ammoniacal liquor regulator solution is 7 then, obtains the mixed solution of reddish-brown.The mixed solution of this reddish-brown at first forms colloidal sol 50 ℃ of heated and stirred, then temperature is risen to 70～80 ℃ and makes colloidal sol form gel, and dry 24h forms xerogel in 80～90 ℃ of baking ovens again.It is segmentation roasting under 860 ℃ of conditions that xerogel is inserted in the retort furnace in top temperature: the fs: 36～250 ℃, and 5 ℃/min of temperature rise rate; Subordinate phase: 250～500 ℃, 7 ℃/min of temperature rise rate; Phase III: 500～860 ℃, 10 ℃/min of temperature rise rate, 860 ℃ of following constant temperature 2 hours.Get nanometer strontium ferrite magnetic powder.By the O-H absorption peak (3000～3500cm that contains in the visible xerogel of Fig. 1-a from tartrate and polyoxyethylene glycol
-1) and the absorption peak 1638cm of C=O
-1, 1384cm
-1Be NO
3 -The eigen vibration absorption peak, 1112cm
-1Stretching vibration absorption peak for C-O-C.Fig. 1-b as can be seen, xerogel is 1384～3500cm after 860 ℃ of roastings
-1Between organism charateristic avsorption band number obviously reduce, and absorption peak strength obviously reduces, and illustrates that organism decomposes substantially fully.And at 400～800cm
-1The absorption of vibrations band of strontium ferrites appears in the place, and peak shape is more sharp-pointed, shows that strontium ferrites forms.XRD spectra among Fig. 2 and SrFe
12O
19PDF standard card (card number: 79-1412) contrast shows: in top temperature is the sample after the segmentation roasting under 860 ℃ of conditions, a large amount of SrFe occurs
12O
19Phase, and the peak all compares sharply, and crystallization is relatively good, non magnetic α-Fe also do not occur
2O
3Phase is single strontium ferrites SrFe substantially
12O
19Phase.The grain-size of gained nanometer strontium ferrite magnetic powder is 20～45nm; Saturation magnetization Ms is 61.330emu/g; HCJ is 4408.2G (seeing Fig. 3 for details).
The preparation of embodiment 2 nanometer strontium ferrite magnetic powders
Taking by weighing 20.1965g iron nitrate crystal is Fe (NO
3)
39H
2O is dissolved in the 50ml deionized water, takes by weighing 0.6151g Strontium carbonate powder (SrCO
3) drip a small amount of salpeter solution until dissolving fully, with Strontium carbonate powder lysate and iron nitrate solution mixing and stirring.Sr and Fe mol ratio are 1: 12 in the above-mentioned mixed solution.8.1337g tartrate is dissolved in the mixed solution, adds 0.6104g polyoxyethylene glycol-2000 stirring and dissolving again after treating to dissolve fully.PH value with the ammoniacal liquor regulator solution is 7 then, obtains the mixed solution of reddish-brown.At first the mixed solution 50 ℃ of heated and stirred reddish-brown forms colloidal sol, then temperature is risen to 70～80 ℃ and makes colloidal sol form gel, and dry 24h forms xerogel in 80～90 ℃ of baking ovens again.It is segmentation roasting under 1100 ℃ of conditions that xerogel is inserted in the retort furnace in top temperature: the fs: 23～320 ℃, and 5 ℃/min of temperature rise rate; Subordinate phase: 320～650 ℃, 7 ℃/min of temperature rise rate; Phase III: 650～1100 ℃, 10 ℃/min of temperature rise rate, 1100 ℃ of following constant temperature 2 hours.Get nanometer strontium ferrite magnetic powder.Fig. 4 is for being the XRD spectra of the sample of segmentation roasting under 1100 ℃ of conditions in top temperature, with SrFe
12O
19PDF standard card (card number: 79-1412) contrast shows, is mainly strontium ferrites SrFe
12O
19Phase.The grain-size of gained nanometer strontium ferrite magnetic powder is: 20～50nm; Saturation magnetization Ms is 78.40emu/g, and HCJ is 3163.3G (seeing Fig. 5 for details).
In the above-mentioned test, can be 1.0～1.5g/100ml, all can realize the preparation of nano-magnetic strontium ferrites the debugging of polyoxyethylene glycol concentration.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although invention has been described by the preferred embodiment with reference to present method, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (5)
1. the preparation method of nanometer strontium ferrite magnetic powder is characterised in that, may further comprise the steps:
The a preparation of raw material: by Sr and Fe mol ratio is 1: 12, and taking by weighing Strontium carbonate powder and iron nitrate crystal is Fe (NO
3)
39H
2O, with nitric acid and deionized water dissolving, mixing back adding tartrate and polyoxyethylene glycol is 7 with ammoniacal liquor adjusting pH, makes mixed solution; Used tartaric mole number is equivalent to Strontium carbonate powder and iron nitrate crystal mole number sum 1 times;
The preparation of b xerogel: step a gained mixed solution is heated into colloidal sol, further is heated into gel, will get xerogel behind the gained gel drying;
The preparation of c nanometer strontium ferrite magnetic powder: is to carry out the segmentation roasting under 860 ℃～1100 ℃ conditions with step b gained xerogel in top temperature, gets nanometer strontium ferrite magnetic powder, and its molecular composition is SrFe
12O
19
2. the preparation method of nanometer strontium ferrite magnetic powder according to claim 1, it is characterized in that: polyoxyethylene glycol described in the step a is a polyoxyethylene glycol-2000, its concentration in mixed solution is 1.0g～1.5g/100ml.
3. the preparation method of nanometer strontium ferrite magnetic powder according to claim 1, it is characterized in that: step b is to be heated into colloidal sol under 50 ℃ with described mixed solution in temperature, is to be heated into gel under 70～80 ℃ of conditions in temperature.
4. according to the preparation method of claim 1,2 or 3 described nanometer strontium ferrite magnetic powders, it is characterized in that: step c is to carry out the segmentation roasting under 860 ℃ of conditions with xerogel in top temperature, and being specially the fs is 36～250 ℃, 5 ℃/min of temperature rise rate; Subordinate phase is 250～500 ℃, 7 ℃/min of temperature rise rate; Phase III is 500～860 ℃, 10 ℃/min of temperature rise rate, again in 860 ℃ of constant temperature 2 hours, nanometer strontium ferrite magnetic powder, it consists of SrFe
12O
19
5. according to the preparation method of claim 1,2 or 3 described nanometer strontium ferrite magnetic powders, it is characterized in that, step c is to carry out the segmentation roasting under 1100 ℃ of conditions with xerogel in top temperature, and be specially: the fs is 23～320 ℃, 5 ℃/min of temperature rise rate; Subordinate phase is 320～650 ℃, 7 ℃/min of temperature rise rate; Phase III is 650～1100 ℃, 10 ℃/min of temperature rise rate, again in 1100 ℃ of constant temperature 2 hours, nanometer strontium ferrite magnetic powder, its molecular formula is SrFe
12O
19
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503392A (en) * | 2011-10-21 | 2012-06-20 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN102807840A (en) * | 2012-08-17 | 2012-12-05 | 中北大学 | Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material |
| CN106830910A (en) * | 2016-12-21 | 2017-06-13 | 马鞍山起劲磁塑科技有限公司 | A kind of preparation method of strontium ferrite magnetic powder |
| CN107151136A (en) * | 2017-05-17 | 2017-09-12 | 马鞍山起劲磁塑科技有限公司 | A kind of preparation method of high-quality injection strontium ferrite magnetic powder |
| CN107324406A (en) * | 2017-07-31 | 2017-11-07 | 电子科技大学 | A kind of composite modified strontium ferrite powder and preparation method thereof |
| CN108686683A (en) * | 2018-05-22 | 2018-10-23 | 重庆大学 | A kind of preparation method of graphene/bismuth oxychloride/cobalt improved strontium ferrite composite photo-catalyst |
| CN109367060A (en) * | 2018-12-10 | 2019-02-22 | 中南大学 | A kind of microwave heating curing method of pair of composite material |
| CN110591218A (en) * | 2019-09-30 | 2019-12-20 | 江苏润集科技有限公司 | Electromagnetic shielding cable material and preparation method thereof |
| CN111974407A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Method for preparing magnetic tungsten trioxide composite photocatalyst |
| CN114771045A (en) * | 2022-05-18 | 2022-07-22 | 成都三洪高科科技有限公司 | Wave-absorbing composite carbon fiber plate |
-
2010
- 2010-08-18 CN CN 201010255857 patent/CN101913854B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 《物理学报》 20050430 方庆清等 单轴M 型SrFe12-xCrxO19超细粒子结构与磁性研究 第1826－1830页 1-5 第54卷, 第4期 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503392B (en) * | 2011-10-21 | 2013-10-02 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN102503392A (en) * | 2011-10-21 | 2012-06-20 | 武汉理工大学 | Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof |
| CN102807840A (en) * | 2012-08-17 | 2012-12-05 | 中北大学 | Preparation method for nanometer Fe3O4-SrFe12O19 compound wave absorption material |
| CN106830910A (en) * | 2016-12-21 | 2017-06-13 | 马鞍山起劲磁塑科技有限公司 | A kind of preparation method of strontium ferrite magnetic powder |
| CN107151136A (en) * | 2017-05-17 | 2017-09-12 | 马鞍山起劲磁塑科技有限公司 | A kind of preparation method of high-quality injection strontium ferrite magnetic powder |
| CN107324406B (en) * | 2017-07-31 | 2019-09-24 | 电子科技大学 | A kind of composite modified strontium ferrite raw powder's production technology |
| CN107324406A (en) * | 2017-07-31 | 2017-11-07 | 电子科技大学 | A kind of composite modified strontium ferrite powder and preparation method thereof |
| CN108686683A (en) * | 2018-05-22 | 2018-10-23 | 重庆大学 | A kind of preparation method of graphene/bismuth oxychloride/cobalt improved strontium ferrite composite photo-catalyst |
| CN108686683B (en) * | 2018-05-22 | 2021-02-09 | 重庆大学 | Preparation method of graphene/bismuth oxychloride/cobalt modified strontium ferrite composite photocatalyst |
| CN109367060A (en) * | 2018-12-10 | 2019-02-22 | 中南大学 | A kind of microwave heating curing method of pair of composite material |
| CN110591218A (en) * | 2019-09-30 | 2019-12-20 | 江苏润集科技有限公司 | Electromagnetic shielding cable material and preparation method thereof |
| CN111974407A (en) * | 2020-07-13 | 2020-11-24 | 重庆大学 | Method for preparing magnetic tungsten trioxide composite photocatalyst |
| CN114771045A (en) * | 2022-05-18 | 2022-07-22 | 成都三洪高科科技有限公司 | Wave-absorbing composite carbon fiber plate |
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