CN102503392A - Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof - Google Patents
Single-phase multi-ferreous strontium-ferrite ceramic material and preparation method thereof Download PDFInfo
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- CN102503392A CN102503392A CN2011103211763A CN201110321176A CN102503392A CN 102503392 A CN102503392 A CN 102503392A CN 2011103211763 A CN2011103211763 A CN 2011103211763A CN 201110321176 A CN201110321176 A CN 201110321176A CN 102503392 A CN102503392 A CN 102503392A
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Abstract
The invention relates to a single-phase multi-ferreous strontium-ferrite ceramic material and a preparation method thereof. The preparation method comprises the following steps: (1) weighing strontium salt and iron salt, forming a precursor solution of strontium and a precursor solution of iron, weighing polyethylene glycol and dissolving in deionized water for standby application; mixing the precursor solutions, stirring, adding the mixed liquid of ammonia and the polyethylene glycol and mixing so as to obtain a suspended solution; centrifugalizing, pouring off liquid at an upper layer, washing precipitates which are centrifugalized out, also calcining and removing organic substances so as to obtain an initial powder body; and grinding, also tabletting and then sintering at high temperature so as to obtain a target product. The single-phase multi-ferreous strontium-ferrite ceramic material and the preparation method thereof have the beneficial effects that the prepared strontium-ferrite ceramic material has multi-ferreous property; meanwhile, the single-phase multi-ferreous strontium-ferrite ceramic material has very good ferroelectricity and ferromagnetism at room temperature; and the single-phase multi-ferreous strontium-ferrite ceramic material and the preparation method thereof have the advantages of simple preparation process, low equipment requirement, easy acquirement of raw materials, low price, small influence to the environment and the like.
Description
Technical field
The present invention relates to a kind of single-phase many iron property strontium ferrite stupalith and preparation method thereof.
Background technology
Performances such as ferroelectric, the ferromagnetic and iron bullet of multi-ferroic material collection are one; Has the coupling between unique many (power, electricity, magnetic, light and heat); Demonstrating a lot of important coupling performances, like magnetoelectricity, piezoelectricity, pyroelectricity and piezomagnetism etc., is important advanced function material.The coupling performance of these materials is that designs provides very big degree of freedom; Make them can be developed into all kinds of transmitters, transverter, driving mechanism and message memory; Be applied to technical fields such as space flight, automotive industry, biology, medical science, information, caused in the world widely and paid close attention to.
Hexagonal strontium ferrite with magnetoplumbite structure is low and have that higher magnetic is long-pending to become one of the most frequently used oxide compound permanent magnet gradually because of its preparation cost.Because strontium ferrite intrinsic crystalline structure has determined it to have characteristics such as high Curie temperature, bigger saturation magnetization, good chemicalstability and erosion resistance, thereby has caused the extensive concern of people to strontium ferrite.
At room temperature having ferroelectricity (810 ℃ of Tc) and weak antiferromagnetism (380 ℃ of Neel temperatures) according to document public reported ferrous acid bismuth, is a kind of multi-ferroic material that has and have magneto-electric coupled character simultaneously because of the ferroelectricity that causes in order and the magnetic of structural parameter.But because the big leakage conductance of ferrous acid bismuth makes its ferroelectricity at room temperature be difficult to saturated polarization, big limitations its application.Therefore how to find that a kind of at room temperature to have the multi-ferroic material that bigger ferroelectric and ferromegnetism also can substitute the ferrous acid bismuth simultaneously be the problem that needs most solution at present.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned prior art a kind of single-phase many iron property strontium ferrite stupalith and preparation method thereof to be provided, and many iron of strontium ferrite property stupalith of preparing with this method at room temperature has extraordinary ferroelectricity and ferromegnetism simultaneously.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: single-phase many iron property strontium ferrite stupalith is characterized in that its chemical formula is: SrFe
12O
19, hexagonal system, spacer: P63/mmc; Molecular weight: 1061.7486, described single-phase many iron property strontium ferrite stupalith at room temperature has good ferroelectric property and ferromegnetism simultaneously, and crystal grain is evenly distributed; Average crystal grain: 1 ~ 5mm, color and luster: black is to garnet.
The preparation method of described single-phase many iron property strontium ferrite stupalith includes following steps:
1) take by weighing strontium salt, molysite according to mol ratio 1:8 ~ 1:12, wherein strontium salt is dissolved in the deionized water, forms the precursor solution of strontium, and iron salt dissolved forms the precursor solution of iron in deionized water, take by weighing polyoxyethylene glycol and be dissolved in the deionized water, and is subsequent use;
2) precursor solution of the precursor solution of the strontium of step 1) gained and iron is mixed stir 1 ~ 2h, add the mixed solution of ammoniacal liquor and polyoxyethylene glycol, make the precursor solution of strontium and the precursor solution mixing of iron obtain suspension solution;
3) with step 2) suspension solution that obtains carries out centrifugally, outwells upper strata liquid, with the centrifugal washing of precipitate that goes out and calcine, removes organism, obtains initial powder;
4) the initial powder that step 3) is obtained grinds and compressing tablet, carries out high temperature sintering again, obtains title product.
Press such scheme, described strontium salt is strontium nitrate or strontium chloride.
Press such scheme, described molysite is ferric acetyl acetonade, iron nitrate or iron(ic)chloride.
Press such scheme, the molecular weight of described polyoxyethylene glycol is 2000 ~ 20000.
Press such scheme, the described calcining concrete steps of step 3) are: the heat-up rate with 2 ~ 10 ℃/min rises to 350 ~ 500 ℃ from room temperature, and at 350 ~ 500 ℃ of insulation 1 ~ 3h, then nature cools to room temperature then.
Press such scheme; The described sintering concrete steps of step 4) are: the heat-up rate with 2 ~ 15 ℃/min rises to 900 ~ 1000 ℃ from room temperature; Then the heat-up rate with 2 ~ 8 ℃/min rises to 1100 ℃ ~ 1400 ℃ from 900 ~ 1000 ℃; Then at this temperature insulation 1 ~ 5h, reduce to 300 ~ 600 ℃ and naturally cool to room temperature with the cooling rate of 2 ~ 8 ℃/min again.
Ultimate principle of the present invention is: after the precursor solution of strontium and the precursor solution of iron mix, add ammoniacal liquor and form strontium hydroxide and ferric hydroxide precipitate, belong to ionic reaction; Centrifugally go out throw out, calcine at 450 ℃, strontium hydroxide and ironic hydroxide are decomposed into strontium oxide and red stone respectively, belong to decomposition reaction; Carry out sintering at 1100 ℃ ~ 1400 ℃ then, strontium oxide and red stone generate strontium ferrite according to certain molar ratio generation solid state reaction, belong to solid state reaction.
Beneficial effect of the present invention is: prepared strontium ferrite stupalith has many iron property, at room temperature has extraordinary ferroelectricity and ferromegnetism simultaneously, and through test, the residual electric polarization of strontium ferrite stupalith is 37.4 μ C/cm
2, coercive electric field is 32kV/m, and remanent magnetic polarization is 34emu/g, and coercive field is 4180Oe, and the both is than the BiFeO that has reported
3Pottery big many, the residual electric polarization of strontium ferrite stupalith is BiFeO
3The pottery 6.13 times.It is reported BiFeO
3The remanent magnetic polarization and the coercive field of pottery are respectively 0.1emu/g and 200Oe, with BiFeO
3The ceramic phase ratio, the remanent magnetic polarization of strontium ferrite stupalith is BiFeO
3The pottery 340 times, coercive field is BiFeO
3The pottery 20.9 times.Single-phase strontium ferrite (SrFe
12O
19) stupalith at room temperature has very good ferroelectric property and ferromegnetism simultaneously, have tangible many iron characteristic, but be a kind of single-phase multi-ferroic material of practicability.In addition, the present invention has that preparation technology is simple, equipment requirements is low, raw material is easy to get and low price, to advantages such as environmental influence are little.
Description of drawings
Fig. 1 is the XRD figure spectrum of the strontium ferrite material that makes of the embodiment of the invention 1;
Fig. 2 is the strontium ferrite material ferroelectric hysteresis loop figure at room temperature that the embodiment of the invention 1 makes;
Fig. 3 is the strontium ferrite material magnetic hysteresis loop figure at room temperature that the embodiment of the invention 1 makes.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed explanation.
According to the Sr/Fe ratio be 1:10 respectively weighing strontium nitrate 0.2127g be dissolved in the 20ml deionized water, weighing iron nitrate 4.1017g is dissolved in the 20ml deionized water, simultaneously (molecular weight: 20000) 1g is dissolved in the 20ml deionized water subsequent use the weighing polyoxyethylene glycol.The precursor solution of the precursor solution of the strontium that obtains and iron mixed stir 2h, add the aqueous solution and the ammoniacal liquor 100ml of polyoxyethylene glycol and 50 ℃ of thorough mixing regular hours.With the outstanding turbid solution centrifugal that obtains; The centrifugal deposition that goes out places corundum crucible to remove organism at 450 ℃ of sintering 1.5h earlier; The sintering concrete steps are: the heat-up rate with 5 ℃/min rises to 450 ℃ from room temperature, and then 450 ℃ of insulation 1.5h, and then nature cools to room temperature.Then grinding also, compressing tablet sinters pottery at 1100 ℃; Described sintering concrete steps are: the heat-up rate with 10 ℃/min rises to 1000 ℃ from room temperature; Then the heat-up rate with 5 ℃/min rises to 1100 ℃ from 1000 ℃; Then at this temperature insulation 1h, reduce to 500 ℃ and naturally cool to room temperature with the cooling rate of 8 ℃/min from sintering temperature again.Not having dephasign in the strontium ferrite stupalith that obtains, is pure single-phase, and its remnant polarization is 37.4 μ C/cm
2, coercive electric field is 32kV/m, and remanent magnetic polarization is 34emu/g, and saturated pole intensity is 60emu/g, and coercive field is 4180Oe.The XRD figure spectrum of the strontium ferrite material that the present invention as shown in Figure 1 makes; As can be seen from the figure, the strontium ferrite that the present invention makes is pure single-phase strontium ferrite stupalith, and its structure is a hexagonal structure, phase free from foreign meter.Fig. 2 is the strontium ferrite material ferroelectric hysteresis loop figure at room temperature that the present invention makes; As can be seen from the figure, the remnant polarization of the strontium ferrite stupalith that makes of the present invention is 37.4 μ C/cm
2, coercive electric field is 32kV/m.Analysis through to crystalline structure finds in six sides' that the present invention prepares strontium ferrite crystalline structure, to exist iron oxygen octahedra perovskite structure; In normal octahedron; The iron cation-bit is in octahedral center that oxygen anion constitutes, yet, in the strontium ferrite that the present invention prepares; Find that the iron positively charged ion has departed from the position at octahedra center; Distortion has taken place, and asymmetrical octahedron is the root that produces electric dipole moment, also is the reason that causes the spontaneous polarization under the extra electric field effect of strontium ferrite stupalith.Therefore, the single-phase strontium ferrite for preparing of the present invention has the ferroelectricity of intrinsic.Fig. 3 is the strontium ferrite material magnetic hysteresis loop figure at room temperature that the present invention makes, and as can be seen from the figure, the remanent magnetic polarization of the strontium ferrite stupalith that the present invention makes is 34emu/g, and saturated pole intensity is 60emu/g, and coercive field is 4180Oe.Strontium ferrite is traditional magneticsubstance, and its magnetic performance is by extensive studies, and magnetic derives from the spin magnetic moment of iron atom.
Embodiment 2
According to the Sr/Fe ratio be 1:8.5 respectively weighing strontium chloride 0.4254g be dissolved in the 20ml deionized water; Weighing iron nitrate 8.2034g is dissolved in the 20ml deionized water, and (molecular weight: 10000) 1g is dissolved in the 20ml deionized water subsequent use the polyoxyethylene glycol of weighing simultaneously.The precursor solution of the precursor solution of the strontium that obtains and iron mixed stir 2h, add the aqueous solution and the ammoniacal liquor 100ml of polyoxyethylene glycol and 50 ℃ of thorough mixing for some time.With the outstanding turbid solution centrifugal that obtains; The centrifugal deposition that goes out places corundum crucible to remove organism at 350 ℃ of sintering 3h earlier; The sintering concrete steps are: the heat-up rate with 5 ℃/min rises to 350 ℃ from room temperature, and then 350 ℃ of insulation 3h, and then nature cools to room temperature.Then grinding also, compressing tablet sinters pottery at 1200 ℃; Described sintering concrete steps are: the heat-up rate with 10 ℃/min rises to 950 ℃ from room temperature; Then the heat-up rate with 5 ℃/min rises to 1200 ℃ from 950 ℃; Then at this temperature insulation 1h, reduce to 400 ℃ and naturally cool to room temperature with the cooling rate of 8 ℃/min from sintering temperature again.Not having dephasign in the strontium ferrite stupalith that obtains, is pure single-phase compound, and its remnant polarization is 37.4 μ C/cm
2, coercive electric field is 32kV/m, and remanent magnetic polarization is 34emu/g, and saturated pole intensity is 60emu/g, and coercive field is 4180Oe.
Embodiment 3
According to the Sr/Fe ratio be 1:11.5 respectively weighing strontium nitrate 0.4254g be dissolved in the 20ml deionized water; Weighing iron nitrate 8.2034g is dissolved in the 20ml deionized water, and (molecular weight: 2000) 1g is dissolved in the 20ml deionized water subsequent use the polyoxyethylene glycol of weighing simultaneously.The precursor solution of the precursor solution of the strontium that obtains and iron mixed stir 2h, add the aqueous solution and the ammoniacal liquor 100ml of polyoxyethylene glycol and 50 ℃ of thorough mixing regular hours.With the outstanding turbid solution centrifugal that obtains; The centrifugal deposition that goes out places corundum crucible to remove organism at 400 ℃ of sintering 2h earlier; The sintering concrete steps are: the heat-up rate with 5 ℃/min rises to 400 ℃ from room temperature, and then 400 ℃ of insulation 2h, and then nature cools to room temperature.Then grinding also, compressing tablet sinters pottery at 1350 ℃; Described sintering concrete steps are: the heat-up rate with 10 ℃/min rises to 900 ℃ from room temperature; At this temperature insulation 1h; Then rise to 1350 ℃ from 900 ℃,, reduce to 300 ℃ and naturally cool to room temperature with the cooling rate of 8 ℃/min from sintering temperature more then at this temperature insulation 1h with the heat-up rate of 5 ℃/min.Not having dephasign in the strontium ferrite stupalith that obtains, is pure single-phase.Its remnant polarization is 16 μ C/cm
2, coercive electric field is 14kV/m.
Claims (7)
1. single-phase many iron property strontium ferrite stupalith is characterized in that its chemical formula is: SrFe
12O
19, hexagonal system, spacer: P63/mmc; Molecular weight: 1061.7486; Described single-phase many iron property strontium ferrite stupalith at room temperature has good ferroelectric property and ferromegnetism simultaneously, and crystal grain is evenly distributed, average crystal grain: 1 ~ 5mm; Color and luster: black has ferroelectricity and ferromagnetic single-phase barium ferrite (BaFe in the future simultaneously to garnet
12O
19) material is applied to many iron property field, like many iron property electronic devices and components, many iron property holder etc. are all in the claim scope of this patent.
2. the preparation method of the described single-phase many iron property strontium ferrite stupalith of claim 1 is characterized in that including following steps:
1) take by weighing strontium salt, molysite according to mol ratio 1:8 ~ 1:12, wherein strontium salt is dissolved in the deionized water, forms the precursor solution of strontium, and iron salt dissolved forms the precursor solution of iron in deionized water, take by weighing polyoxyethylene glycol and be dissolved in the deionized water, and is subsequent use;
2) precursor solution of the precursor solution of the strontium of step 1) gained and iron is mixed stir 1 ~ 2h, add the mixed solution of ammoniacal liquor and polyoxyethylene glycol, make the precursor solution of strontium and the precursor solution mixing of iron obtain suspension solution;
3) with step 2) suspension solution that obtains carries out centrifugally, outwells upper strata liquid, with the centrifugal washing of precipitate that goes out and calcine, removes organism, obtains initial powder;
4) the initial powder that step 3) is obtained grinds and compressing tablet, carries out high temperature sintering again, obtains title product.
3. by the preparation method of the described single-phase many iron property strontium ferrite stupalith of claim 2, it is characterized in that described strontium salt is strontium nitrate or strontium chloride.
4. by the preparation method of the described single-phase many iron property strontium ferrite stupalith of claim 2, it is characterized in that described molysite is ferric acetyl acetonade, iron nitrate or iron(ic)chloride.
5. by the preparation method of claim 2 or 3 or 4 described single-phase many iron property strontium ferrite stupaliths, the molecular weight that it is characterized in that described polyoxyethylene glycol is 2000 ~ 20000.
6. press the preparation method of claim 2 or 3 or 4 described single-phase many iron property strontium ferrite stupaliths; It is characterized in that the described calcining concrete steps of step 3) are: the heat-up rate with 2 ~ 10 ℃/min rises to 350 ~ 500 ℃ from room temperature; At 350 ~ 500 ℃ of insulation 1 ~ 3h, then nature cools to room temperature then.
7. press the preparation method of the described single-phase many iron property strontium ferrite stupalith of claim 6; It is characterized in that the described sintering concrete steps of step 4) are: the heat-up rate with 2 ~ 15 ℃/min rises to 900 ~ 1000 ℃ from room temperature; Then the heat-up rate with 2 ~ 8 ℃/min rises to 1100 ℃ ~ 1400 ℃ from 900 ~ 1000 ℃; Then at this temperature insulation 1 ~ 5h, reduce to 300 ~ 600 ℃ and naturally cool to room temperature with the cooling rate of 2 ~ 8 ℃/min again.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787420A (en) * | 2014-01-25 | 2014-05-14 | 陕西科技大学 | Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method |
| CN107032776A (en) * | 2016-11-22 | 2017-08-11 | 武汉理工大学 | Single-phase multiferroic M types strontium ferrite ceramics and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103787420A (en) * | 2014-01-25 | 2014-05-14 | 陕西科技大学 | Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method |
| CN107032776A (en) * | 2016-11-22 | 2017-08-11 | 武汉理工大学 | Single-phase multiferroic M types strontium ferrite ceramics and preparation method thereof |
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