CN101920999B - Method for preparing nano strontium ferrite - Google Patents
Method for preparing nano strontium ferrite Download PDFInfo
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- CN101920999B CN101920999B CN2010102381940A CN201010238194A CN101920999B CN 101920999 B CN101920999 B CN 101920999B CN 2010102381940 A CN2010102381940 A CN 2010102381940A CN 201010238194 A CN201010238194 A CN 201010238194A CN 101920999 B CN101920999 B CN 101920999B
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Abstract
The invention discloses a method for preparing nano strontium ferrite, which comprises the following steps of: mixing strontium nitrate, ferric nitrate, sodium nitrate, potassium nitrate and sodium peroxide; melting the mixture at the temperature of between 400 and 800 DEG C, preserving the heat, and then cooling the mixture to room temperature; and then washing and drying the mixture to obtain a solid product, namely the nano strontium ferrite with distribution size of between 26 to 43nm. The method has the advantages of simple used equipment and process, low reaction temperature, low cost, low energy consumption, small grain of the product, uniform distribution of the particle size, and suitability for industrial production.
Description
Technical field
The invention belongs to the perovskite material preparing technical field, particularly a kind of preparation method of nano strontium ferrite.
Background technology
Strontium ferrite is a kind of important perovskite compound, this be since in the strontium ferrite valence state of iron be+4, the valence electron of iron ion is configured as 3d
4(t
2g 3e
g 1), very unstable, electron transport takes place in the process that forms calcium titanium ore structure easily, form the 3d electronics and reach the Fe that partly is full of
3+,, can produce a large amount of oxygen rooms in the crystal, thereby strontium ferrite can be widely used in aspects such as catalyzer, battery, gas sensor, magnet for keeping the whole electroneutral of crystal.
The method for preparing at present the nano strontium ferrite material mainly contains solid-phase synthesis, hydrothermal method, combustion method, coprecipitation method and sol-gel method etc.There are some shortcomings in these existing preparing methods, need the pyroreaction more than the 1100K like the solid-phase synthesis of employings such as Zyryanov; The hydrothermal method that Wang etc. adopt needs 25 atmospheric high pressure; The combustion method that Ming etc. adopt need keep 5 hours at 1500 ℃ of high temperature; The coprecipitation method that Augustin etc. adopt needs 3.5 tons/square metre pressure and 1000 ℃ high temperature; The sol-gel method that Song and Majid etc. adopt, preparation process is many, complicated operation, and need more than 600 ℃ temperature roasting etc. at least.It is thus clear that existing preparation method generally needs higher preparation temperature.
Summary of the invention
The technical problem that the present invention will solve is the shortcoming to existing preparation nano strontium ferrite method, provide a kind of low for equipment requirements, technology is simple, easy and simple to handle, cost is low, energy consumption is low, obtain the preparation method of the little nano level ferrous acid strontium of crystal grain.This preparation method is a molten-salt growth method.
The present invention adopts following scheme to realize: a kind of preparation method of nano level ferrous acid strontium may further comprise the steps:
(1) with nitrate salt and sodiumperoxide mixing; Described nitrate salt is strontium nitrate, iron nitrate, SODIUMNITRATE and saltpetre 1: 1 in molar ratio: (10～30): formation is mixed in (10～30);
(2) mixture that step (1) is obtained is in 400～800 ℃ of fusings, and insulation is cooled to room temperature then, and the solid product that obtains after the washing drying is nano level ferrous acid strontium.
Nitrate salt and sodiumperoxide described in the step (1) are 11～31: 1 mixing in molar ratio;
The mixture that said step (2) more preferably obtains step (1) is in 400～800 ℃ of fusings, and insulation is cooled to room temperature then, and with deionized water wash, drying, the solid product that obtains is nano level ferrous acid strontium;
Keeping of insulation is preferably 2～48h described in the step (2);
The device of fusing is preferably retort furnace described in the step (2);
The exsiccant temperature is preferably 80 ℃ described in the step (2).
The present invention has following advantage and effect with respect to prior art:
The present invention is through using existing nitrate salt and sodiumperoxide; Through control different heating temperature and soaking time; Finally obtain nano level strontium ferrite powder; Equipment and the technology that this process is used is simple, temperature of reaction is low, cost is low, energy consumption is low, product crystal grain is little (be 26～43nm), and particle size dispersion is even, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 1.
Fig. 2 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 1.
Fig. 3 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 2.
Fig. 4 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 2.
Fig. 5 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 3.
Fig. 6 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 3.
Fig. 7 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 4.
Fig. 8 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 4.
Fig. 9 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 5.
Figure 10 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 5.
Figure 11 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 6.
Figure 12 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 6.
Figure 13 is the X-ray diffractogram of the nano level ferrous acid strontium for preparing of embodiment 7.
Figure 14 is the awkward silence at a meeting emission scan Electronic Speculum figure of the nano level ferrous acid strontium for preparing of embodiment 7.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1
(1) gets 2.000g strontium nitrate, 3.818g iron nitrate, 4.016g SODIUMNITRATE, 4.777g saltpetre and 1.474g sodiumperoxide and mix (SODIUMNITRATE, the mol ratio of saltpetre and sodiumperoxide is 1: 1: 10: 10: 2 for strontium nitrate, iron nitrate).
(2) mixture that step (1) is obtained is positioned in the retort furnace; Keep 24h in 400 ℃, naturally cool to room temperature then, with obtaining solid product through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains is through X-ray diffraction (siemens D-5000 diffractometer, the monochromatic diffraction K of copper target
α 1(the voltage 40kV of λ=0.15405nm); Electric current 30mA; 0.01 ° of step-length .) and awkward silence at a meeting emission scan Electronic Speculum (SEM, JEOL JSM-6330F) detection, can know that the crystal that obtains is that size is the nano level ferrous acid strontium (as depicted in figs. 1 and 2) of 33nm (PDF standard card number: 34-0641); Narrow particle size distribution, i.e. uniform particles.
Embodiment 2
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 450 ℃ of maintenance 6h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 34nm (like Fig. 3 and shown in Figure 4, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
Embodiment 3
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 450 ℃ of maintenance 24h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 34nm (like Fig. 5 and shown in Figure 6, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
Embodiment 4
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 450 ℃ of maintenance 48h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 32nm (like Fig. 7 and shown in Figure 8, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
Embodiment 5
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 500 ℃ of maintenance 24h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 41nm (like Fig. 9 and shown in Figure 10, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
Embodiment 6
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 600 ℃ of maintenance 2h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 41nm (like Figure 11 and shown in Figure 12, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
Embodiment 7
(1) with embodiment 1 step (1)
(2) mixture that step (1) is obtained is positioned in the retort furnace, in 600 ℃ of maintenance 24h, naturally cools to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings; The crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 36nm (like Figure 13 and shown in Figure 14, testing method is with embodiment 1); Narrow particle size distribution, i.e. uniform particles.
(1) gets 2.000g strontium nitrate, 3.818g iron nitrate, 12.048g SODIUMNITRATE, 14.331g saltpetre and 1.474g sodiumperoxide and mix (SODIUMNITRATE, the mol ratio of saltpetre and sodiumperoxide is 1: 1: 20: 20: 2 for strontium nitrate, iron nitrate).
(2) mixture that step (1) is obtained is positioned in the retort furnace; Keep 24h in 450 ℃; Slowly cool to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings, the crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 34nm.
Embodiment 9
(1) gets 2.000g strontium nitrate, 3.818g iron nitrate, 12.048g SODIUMNITRATE, 14.331g saltpetre and 1.474g sodiumperoxide and mix (SODIUMNITRATE, the mol ratio of saltpetre and sodiumperoxide is 1: 1: 30: 30: 2 for strontium nitrate, iron nitrate).
(2) mixture that step (1) is obtained is positioned in the retort furnace; Keep 24h in 450 ℃; Slowly cool to room temperature then; To heat the back solid product that obtains through deionized water wash, in 80 ℃ of dryings, the crystal grain that obtains detects through X-ray diffraction and awkward silence at a meeting emission scan Electronic Speculum, can know that the crystal that obtains is that size is the nano level ferrous acid strontium of 36nm.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. the preparation method of a nano level ferrous acid strontium is characterized in that may further comprise the steps:
(1) with nitrate salt and sodiumperoxide mixing; Described nitrate salt is strontium nitrate, iron nitrate, SODIUMNITRATE and saltpetre 1:1 in molar ratio: (10～30): formation is mixed in (10～30);
(2) mixture that step (1) is obtained is in 400～800 ℃ of fusings, and insulation is cooled to room temperature then, and the solid product that obtains after the washing drying is nano level ferrous acid strontium;
Nitrate salt and sodiumperoxide described in the step (1) are to be that 11～31:1 mixes in molar ratio.
2. according to the preparation method of the said nano level ferrous acid of claim 1 strontium; It is characterized in that: said step (2) for mixture that step (1) is obtained in 400～800 ℃ of fusings; Insulation; Be cooled to room temperature then, with deionized water wash, drying, the solid product that obtains is nano level ferrous acid strontium.
3. according to the preparation method of the said nano level ferrous acid of claim 2 strontium, it is characterized in that: said exsiccant temperature is 80 ℃.
4. according to the preparation method of each said nano level ferrous acid strontium of claim 1～3, it is characterized in that: the time of insulation is 2～48 h described in the step (2).
5. according to the preparation method of each said nano level ferrous acid strontium of claim 1～3, it is characterized in that: the device of fusing is a retort furnace described in the step (2).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030077382A1 (en) * | 1998-11-06 | 2003-04-24 | Yang-Ki Hong | Substantially spherical magneto-plumbite ferrite particles and methods for producing and media employing the same |
| 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 |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030077382A1 (en) * | 1998-11-06 | 2003-04-24 | Yang-Ki Hong | Substantially spherical magneto-plumbite ferrite particles and methods for producing and media employing the same |
| 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 (3)
| Title |
|---|
| Si-Dong Kim et al..Magnetic properties of Sr-ferrites synthesized in molten (NaCl+KCl) flux.《Journal of Magnetism and Magnetic Materials》.2006,第307卷第295-300页. * |
| 康振晋.共沉淀法合成铁酸锶及其光催化活性研究.《延边大学学报(自然科学版)》.2005,第31卷(第4期), * |
| 桑丽霞等.LaFeO 3和SrFeO 3-λ 对水溶性染料的光催化降解.《环境科学与技术》.2002,第25卷(第2期), * |
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