CN101209921A - Method for preparing single-phase Y-doping bismuth ferrate magnetoelectric ceramic - Google Patents
Method for preparing single-phase Y-doping bismuth ferrate magnetoelectric ceramic Download PDFInfo
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- CN101209921A CN101209921A CNA2007101440935A CN200710144093A CN101209921A CN 101209921 A CN101209921 A CN 101209921A CN A2007101440935 A CNA2007101440935 A CN A2007101440935A CN 200710144093 A CN200710144093 A CN 200710144093A CN 101209921 A CN101209921 A CN 101209921A
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- bismuth ferrate
- doping bismuth
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Abstract
The invention relates to a preparation method of a single phase Y doped bismuth ferrate magneto-electric ceramics, which relates to the magneto-electric ceramics field; the invention provides a preparation method of a single phase Y doped bismuth ferrate magneto-electric ceramics that can effectively restrain the generation of dephasign, enhance the isolation performance of a sample, with simple production technique, good reproducibility and low cost. The chemical formula of the single phase Y doped bismuth ferrate magneto-electric ceramics is Bi1-xYxFeO3, wherein, x is more than or equal to 0 and less than or equal to 0.1. Materials of bismuth oxide, yttrium oxide and ferric oxide are blended into a mixture according to a general formula Bi1-xYxFeO3 (x is more than or equal to 0 and less than and equal to 0.1) and ball milled, and the obtained slurry is dried, presintered, and the presintered powder material is ball milled for a second time, dried, added with polyvinyl alcohol granulation, sieved and dry pressed for forming, and finally sintered and heat insulated.
Description
Technical field
The present invention relates to a kind of magnetoelectric ceramic, especially relate to a kind of preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic.
Background technology
Ferromagnetic in recent years electric material has caused the great interest of people, it has ferroelectricity and ferromegnetism simultaneously, can induce by electric field and produce magnetization, electropolarization also can be brought out in magnetic field, this character is called as magnetoelectric effect, the mutual control character of this magnetic and electricity aspect information storage, spin electric device, Magnetic Sensor and electric capacity-inductor integrated device, all has extremely important application prospect.For example, utilize the magneto-electric coupled effect of material, the field signal of complexity can be converted to the electrical signal that is easy to measure, effectively monitor the changing conditions in magnetic field, can substitute the hall probe of widely using at present.In addition, mutual control action kou according to magnetic and electricity, might design with quick electropolarization induces the magnetooptical disc of magnetization inversion fast to replace the existing reading and writing memory of magnetic at a slow speed material, this material had both had the advantage of traditional ferroelectric material fast reading and writing, the fatigue phenomenon that ferroelectric material produces because of the electricdomain pinning can be overcome again in polarization reversal, a kind of novel material with memory that integrates the excellent property of ferroelectric material and magneticsubstance advantage may be become.Simultaneously, because ferroelectricity and ferromagnetic coexistence, make this material have high specific inductivity and magnetic permeability simultaneously, utilize this characteristic can make high capacitance and big inductor integrated electronic devices and components, for reducing the number of devices on the high density circuit board, the mutual interference problem that solves perceptual device and capacitive device provides new thinking.In addition, the electricity of this material and the coupling of magnetic parameter also provide possibility for it in the application aspect the spin electric device, and the basic physics aspect that is coupling in of this order parameter also is extremely important.
Ferrous acid bismuth (BiFeO
3) be that minority at room temperature has one of ferroelectricity and ferromagnetic material simultaneously, belong to R3c space point group, Curie temperature is 830 ℃, triangle perovskite structure torsional deformation and cause ferroelectricity is G type antiferromagnetic order in Neel temperature below 370 ℃.Though find BiFeO very early
3In the ferroelectricity and the ferromegnetism of coexistence, but because big leakage conductance can't accurately be measured its ferroelectricity, simultaneously the room temperature magnetic a little less than, these characteristics have limited its application widely.
The BiFeO of traditional solid reaction process preparation
3Pottery is usually with Bi
2Fe
4O
9And Bi
36Fe
2O
57Etc. phase, be difficult to prepare monophasic BiFeO
3Pottery.A lot of for this reason study group are at preparation BiFeO monophasic, that insulating property are good, the ferroelectric property excellence
3A large amount of work has been launched in the pottery aspect, has obtained certain progress.People such as M.Mahesh (M.Mahesh Kumar, etal.Applied Physics Letters (Applied Physics communication) 76,2764 (2004)) adopt earlier traditional solid reaction process preparation contain dephasign BiFeO
3Pottery then with rare nitric acid cleaning dephasign wherein, thereby obtains monophasic BiFeO
3Pottery.(Chinese patent, publication number CN 1686932A) such as the Zhang Shantao of Nanjing University is to agglomerating BiFeO
3Pottery carries out quick cooling process, adopts quench method to prepare single-phase BiFeO
3Pottery.(V.R.Palkar such as Palkar, D.C.Kundaliya, and S.K.Malik, Effect of Mn substitution on magnetoelectric properties of bismuthferrite system.J.Appl.Phys.2003,93 (7) 4337-4339) to BiFeO
3Pottery has carried out the La doping, has obtained certain effect.。Yet Y doping BiFeO
3Pottery yet there are no report, Y
3+With Bi
3+Ionic radius is close, and magnetic is stronger, is preparation single-phase Y-doping BiFeO
3Magnetoelectric ceramic provides may.
Summary of the invention
The purpose of this invention is to provide a kind of generation that can effectively suppress dephasign, improve the insulating property of sample, production technique is simple, favorable reproducibility, single-phase Y-doping bismuth ferrate (BiFeO with low cost
3) preparation method of magnetoelectric ceramic.
The chemical molecular formula of single-phase Y-doping bismuth ferrate magnetoelectric ceramic of the present invention is: Bi
1-xY
xFeO
3, wherein: 0≤x≤0.1.
The preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic of the present invention may further comprise the steps:
1) with raw material bismuth oxide (Bi
2O
3), yttrium oxide (Y
2O
3) and ferric oxide (Fe
2O
3), by prescription Formula B i
1-xY
xFeO
3(0≤x≤0.1) is made into compound, the slurry of gained oven dry behind the ball milling, pre-burning;
2) ball milling once more of the powder after the pre-burning, the oven dry back adds polyvinyl alcohol (PVA) granulation, and the back of sieving is dry-pressing formed, is incubated behind the sintering.
In step 1), the medium of ball milling can be dehydrated alcohol and zirconia ball, and the time of ball milling can be 2～8h, and rotating speed can be 200～400r/min, and the granularity of ball milling is preferably less than 5 μ m; The temperature of slurry oven dry is preferably 80～150 ℃, and described pre-burning can be adopted alumina crucible, and the temperature of pre-burning can be 750～800 ℃, preferably is incubated 2～6h after the pre-burning.
In step 2) in, preferably less than 5 μ m, the concentration of polyvinyl alcohol is preferably 5%～7% to the granularity of ball milling, crosses 40～80 mesh sieves after the granulation, and the dry-pressing formed pressure in back that sieves is preferably 120～200MPa.Sintering can adopt air atmosphere and normal pressure-sintered, and the agglomerating temperature can be 840～880 ℃ flat-temperature zone, and is incubated 1～5h.
From the Bi that different ingredients is prepared
1-xY
xFeO
3The test effect of magnetoelectric ceramic is compared with existing method, and outstanding feature of the present invention is: can prepare monophasic and the good Bi of insulating property
1-xY
xFeO
3Magnetoelectric ceramic.The method that the present invention adopts can suppress the generation of dephasign effectively, improve the insulating property of sample, and production technique is simple, and favorable reproducibility is with low cost.
Description of drawings
The single-phase Y-doping BiFeO that Fig. 1 prepares for the present invention
3The SEM photo of magnetoelectric ceramic.
The single-phase Y-doping BiFeO that Fig. 2 prepares for the present invention
3The XRD spectrum of magnetoelectric ceramic.In Fig. 2, X-coordinate be diffraction angle 2 θ/(°), ordinate zou is diffracted intensity Intensity (a.u.), and diffraction peak is respectively (012) (104) (110) (006) (202) (024) (116) (122) (018) (214) (300) (208) (220) (036) (312) (134) from left to right.
Embodiment
Following examples will the present invention is further illustrated, is noted that the present invention is not limited to following each embodiment.
Material rate, calcined temperature and the sintering temperature of 3 prescriptions that embodiment adopted of the present invention are as shown in table 1.
Table 1
| Embodiment | Raw material Bi 2O 3∶Y 2O 3∶Fe 2O 3(mol ratio) | Calcined temperature/℃ | Sintering temperature/℃ |
| 1 | 0.98∶0.02∶1 | 750 | 840 |
| 2 | 0.96∶0.04∶1 | 770 | 860 |
| 3 | 0.92∶0.08∶1 | 800 | 880 |
Embodiment 1
Fill a prescription weighing Bi according to the above ratio
2O
3, Y
2O
3And Fe
2O
3Be made into compound, the weight ratio by compound and dehydrated alcohol, zirconia ball is 1: 1.2: 2 again, adds dehydrated alcohol and zirconia ball respectively, planetary ball mill 2h, 400r/min, the slurry behind the ball milling is put into alumina crucible at 750 ℃ of following pre-burning 6h 80 ℃ of oven dry down.Powder after the pre-burning is ball milling once more, and adding concentration in oven dry back is 5% PVA granulation, crosses 60 mesh sieves.Granulation material after sieving is dry-pressing formed under the pressure of 180MPa, and sample adopts air atmosphere, normal pressure-sintered, is incubated 5h down at 840 ℃, naturally cools to room temperature then.
Fill a prescription weighing Bi according to the above ratio
2O
3, Y
2O
3And Fe
2O
3Be made into compound, the weight ratio by compound and dehydrated alcohol, zirconia ball is 1: 1.2: 2 again, adds dehydrated alcohol and zirconia ball respectively, planetary ball mill 4h, 300r/min, the slurry behind the ball milling is put into alumina crucible at 770 ℃ of following pre-burning 3h 100 ℃ of oven dry down.Powder after the pre-burning is ball milling once more, and adding concentration in oven dry back is 7% PVA granulation, crosses 80 mesh sieves.Granulation material after sieving is dry-pressing formed under the pressure of 200MPa, and sample adopts air atmosphere, normal pressure-sintered, is incubated 3h down at 860 ℃, naturally cools to room temperature then.
Embodiment 3
Fill a prescription weighing Bi according to the above ratio
2O
3, Y
2O
3And Fe
2O
3Be made into compound, the weight ratio by compound and dehydrated alcohol, zirconia ball is 1: 1.2: 2 again, adds dehydrated alcohol and zirconia ball respectively, planetary ball mill 8h, 250r/min, the slurry behind the ball milling is put into alumina crucible at 800 ℃ of following pre-burning 2h 120 ℃ of oven dry down.Powder after the pre-burning is ball milling once more, and adding concentration in oven dry back is 7% PVA granulation, crosses 40 mesh sieves.Granulation material after sieving is dry-pressing formed under the pressure of 120MPa, and sample adopts air atmosphere, normal pressure-sintered, is incubated 2h down at 880 ℃, naturally cools to room temperature then.
Claims (10)
1. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic is characterized in that the chemical molecular formula of single-phase Y-doping bismuth ferrate magnetoelectric ceramic is: Bi
1-xY
xFeO
3, wherein: 0≤x≤0.1; Its preparation method may further comprise the steps:
1) raw material bismuth oxide, yttrium oxide and ferric oxide are pressed prescription Formula B i
1-xY
xFeO
3(0≤x≤0.1) is made into compound, the slurry of gained oven dry behind the ball milling, pre-burning;
2) ball milling once more of the powder after the pre-burning, the oven dry back adds the polyvinyl alcohol granulation, and the back of sieving is dry-pressing formed, is incubated behind the sintering.
2. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 1), and the medium of ball milling is dehydrated alcohol and zirconia ball.
3. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 1), and the time of ball milling is 2～8h, and rotating speed is 200～400r/min.
4. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 1), and the granularity of ball milling is less than 5 μ m.
5. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 1), and the temperature of slurry oven dry is 80～150 ℃.
6. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 1), and alumina crucible is adopted in described pre-burning, and the temperature of pre-burning is 750～800 ℃, is incubated 2～6h after the pre-burning.
7. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 2) in, the granularity of ball milling is less than 5 μ m.
8. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 2) in, the concentration of polyvinyl alcohol is 5%～7%.
9. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 2) in, cross 40～80 mesh sieves after the granulation, the dry-pressing formed pressure in back that sieves is 120～200MPa.
10. the preparation method of single-phase Y-doping bismuth ferrate magnetoelectric ceramic as claimed in claim 1 is characterized in that in step 2) in, sintering adopts air atmosphere and normal pressure-sintered, and the agglomerating temperature is 840～880 ℃ flat-temperature zone, and is incubated 1～5h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503391A (en) * | 2011-10-20 | 2012-06-20 | 陕西科技大学 | Preparation method of bismuth ferrite-based composite material with high ferromagnetic and ferroelectric properties |
| CN104556238A (en) * | 2014-12-19 | 2015-04-29 | 上海师范大学 | Method for preparing pure-phase bismuth ferrite powder and block |
| CN110002505A (en) * | 2019-05-08 | 2019-07-12 | 东北大学秦皇岛分校 | A kind of preparation method of pure phase nanometer crystalline substance doped yttrium bismuth ferrite |
| CN112537952A (en) * | 2020-12-04 | 2021-03-23 | 安徽工业大学 | Bismuth ferrite-based ceramic with excellent magnetoelectric property and preparation method thereof |
-
2007
- 2007-12-21 CN CNA2007101440935A patent/CN101209921A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503391A (en) * | 2011-10-20 | 2012-06-20 | 陕西科技大学 | Preparation method of bismuth ferrite-based composite material with high ferromagnetic and ferroelectric properties |
| CN104556238A (en) * | 2014-12-19 | 2015-04-29 | 上海师范大学 | Method for preparing pure-phase bismuth ferrite powder and block |
| CN104556238B (en) * | 2014-12-19 | 2016-09-07 | 上海师范大学 | A kind of pure phase bismuth ferric powder and the preparation method of block |
| CN110002505A (en) * | 2019-05-08 | 2019-07-12 | 东北大学秦皇岛分校 | A kind of preparation method of pure phase nanometer crystalline substance doped yttrium bismuth ferrite |
| CN112537952A (en) * | 2020-12-04 | 2021-03-23 | 安徽工业大学 | Bismuth ferrite-based ceramic with excellent magnetoelectric property and preparation method thereof |
| CN112537952B (en) * | 2020-12-04 | 2023-05-09 | 安徽工业大学 | Bismuth ferrite-based ceramic with excellent magnetoelectric performance and preparation method thereof |
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Open date: 20080702 |