CN1603279A - Magneto-electric coupled ceramic materials and preparing method thereof - Google Patents
Magneto-electric coupled ceramic materials and preparing method thereof Download PDFInfo
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- CN1603279A CN1603279A CN200410064900.9A CN200410064900A CN1603279A CN 1603279 A CN1603279 A CN 1603279A CN 200410064900 A CN200410064900 A CN 200410064900A CN 1603279 A CN1603279 A CN 1603279A
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910010293 ceramic material Inorganic materials 0.000 title claims description 14
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 230000015556 catabolic process Effects 0.000 claims abstract description 13
- 230000005684 electric field Effects 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000000704 physical effect Effects 0.000 claims abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 6
- 229910001428 transition metal ion Inorganic materials 0.000 claims abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 230000010287 polarization Effects 0.000 claims description 9
- -1 rare earth cation Chemical class 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 8
- 229910052777 Praseodymium Inorganic materials 0.000 abstract 1
- 229910052772 Samarium Inorganic materials 0.000 abstract 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 7
- 230000005290 antiferromagnetic effect Effects 0.000 description 4
- 230000005294 ferromagnetic effect Effects 0.000 description 4
- 230000005291 magnetic effect Effects 0.000 description 4
- 238000004549 pulsed laser deposition Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 230000005621 ferroelectricity Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000012913 prioritisation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
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Abstract
The invention discloses a magneto-electric coupling ceramics material. Its chemical formula is (Bi1-xAxFe1-yByO3), and 0<=x<0.5, 0<=y<0.2, x, y can not equal 0 in the same time. an is trivalency rare earth metal ion selected one or two kinds from La, Nd, Td, Sm and Pr. B is a transition metal ion Mn or Co. The material has following physical property: breakdown electric field is over 150kV/ cm, its breakdown electric field is between 3 microcoulomb per square centimeter to 30 microcoulomb per square centimeter. Meanwhile, the invention discloses the method to produce the material. Its feature is when sintering, temperature would increase at the speed of 30 degree per second and stabilizing between 850 degree centigrade and 940 degree centigrade, then cooling quickly.
Description
Technical field
The present invention relates to a kind of magneto-electric coupled ceramic materials and preparation method thereof.
Background technology
Ferroelectric magnet or magneto-electric coupled material have ferroelectricity and ferromagnetic (antiferromagnetic) property simultaneously, and can be coupled between ferroelectric electropolarization and ferromagnetic (antiferromagnetic) spin, produce new physical influence, that is to say and to change the magnetic of this class material or by adding the ferroelectricity that magnetic field changes this class material by added electric field.The ferromagnetic Curie temperature of general single-phase ferroelectric magnet is all lower, such as Pb (Nb
1/2Fe
1/2) O
3Ferromagnetic Curie temperature be about-160 ℃.BiFeO
3Be all materials more than room temperature of ferroelectrie Curie temperature (～700 ℃) rare in the existing single-phase ferroelectric magnet and ferromagnetic Curie temperature (～370 ℃).BiFeO
3The antiferromagnetic sinusoidal fluctuation that exists, therefore only have the magneto-electric coupled coefficient of less secondary, but Bi
1-xA
xFe
1-yB
yO
3(0≤x＜0.5,0≤y＜0.2, A is rare earth ion La to series ceramic
3+, Nd
3+, Td
3+, Sm
3+, Pr
3+In one or both, B is a kind of trivalent metal ion Mn
3+Or Co
3+) be expected to destroy antiferromagnetic sinusoidal fluctuation and have the magneto-electric coupled coefficient of bigger one-level.Because BiFeO
3Very responsive to preparation condition, trivalent Fe ionic appraises at the current rate and the volatilization of Bi causes the insulativity of pottery very poor; So before not solving the preparation method, Bi
1-xA
xFe
1-yB
yO
3The research of series ceramic can't effectively be carried out.Current, can successfully prepare high-insulativity (resistivity～10
9Ω cm, breakdown electric field is greater than 150kV/cm) have an ABO
3Type uhligite one-component ceramic is that can this class pottery and film by one of effective development research and optimization and the key factor that is employed.At present, in this field, majority are by general solid-phase sintering method and use Bi
2O
3Powdered preparation Bi
1-xA
xFe
1-yB
yO
3Pottery is so sintering temperature is at Bi
2O
3Fusing point (817 ℃) below.But because trivalent Fe ion appraises at the current rate easily, Bi volatilizees easily, is difficult to obtain pure ABO by general solid-phase sintering method
3To such an extent as to the pottery of phase is thereby the lower ferroelectric hysteresis loop (being the P-V loop line) that can not obtain between saturated electropolarization-electric field of resistivity.
There are two kinds at present specially at BiFeO
3The sintering method of pottery is more famous.First kind is the dephasign of using the ordinary sinter method to form with the nitric acid dissolve of dilution, more remaining pure phase sintering is formed pottery.With the pottery of this method preparation, because be difficult to fully dephasign be removed clean, thereby breakdown electric field still can not reach～150kV/cm, so can't be to BiFeO
3Pottery carries out saturated polarization [M.Mahesh Kumar, V.R.Palkar, K.Srinivas, and S.V.Suryanarayana, Applied Physics Letters76,2764 (2000) .].Second method utilizes NaOH to prepare the oxyhydroxide mixture throw out of desired ion, sinter required powdered material at-550 ℃ then, make ceramic target at last and be used for pulsed laser deposition (PLD) or magnetron sputtering growing film [V.R.Palkar, Darshan C.Kundaliya, and S.K.Malik, Indian Patent Application No.409/MUM/2003, dated 24 April 2003.].At present, there has been the traditional solid-phase sintering method of human to prepare Bi
1-xA
xFe
1-yB
yO
3Series ceramic, but their the ceramic breakdown electric field of preparation is very little, is difficult to measure saturated polarization-electric field loop line [A.V.Zalesskii, A.A.Frolov, T.A.Khimich, and A.A.Bush, Physics of the Solid State45,141 (2003); I.Sosnowska, W.Sch fer, W.Kockelmann, K.H.Andersen, I.O.Troyanchuk, Appl.Phys.A 74, S1040 (2002); V.L.Mathe, K.K.Patankar, R.N.Patil, C.D.Lokhande, Journal of Magnetism and Magnetic Materials270,380 (2004); V.L.Mathe, Journal of Magnetism and Magnetic Materials263,344 (2003) .].The specific performance index of the stupalith of above-mentioned bibliographical information is introduced in Table 1.Therefore, use simple method to prepare resistivity to reach～10
9Ω cm and voltage breakdown are greater than the ABO that has of 150kV/cm
3The Bi of phase structure
1-xA
xFe
1-yB
yO
3, become a urgent task.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that prior art exists, and a kind of magneto-electric coupled ceramic materials Bi is provided
1-xA
xFe
1-yB
yO
3, have following physicals: breakdown electric field is greater than 150kV/cm, and the residual polarization of the polarization of ferroelectric magnet-electric field loop line is at 3-30 μ C/cm
2Between.
Another goal of the invention of the present invention provides the above-mentioned method of ceramic material of a kind of preparation, and the stupalith of contriver's preparation has following physicals: breakdown electric field is greater than 150kV/cm, and the residual polarization of the polarization of ferroelectric magnet-electric field loop line is at 3～30 μ C/cm
2Between.
Above-mentioned physicochemical property is that current material is not available.
Magneto-electric coupled ceramic materials of the present invention is characterized in that:
(1) chemical formula is
Bi
1-xA
xFe
1-yB
yO
3
Wherein: 0≤x＜0.5,0≤y＜0.2 and x, y can not be 0 simultaneously;
A is one or both among rare earth cation La, Nd, Td, Sm, the Pr;
B is a kind of transition metal ion Mn or Co;
(2) has following physicals
Breakdown electric field is greater than 150kV/cm, and the residual polarization of the polarization of ferroelectric magnet-electric field loop line is at 3～30 μ C/cm
2Between.
Prepare above-mentioned method of ceramic material, the steps include:
A) utilize Bi
2O
3, La
2O
3, Fe
2O
3, Td
2O
3, Nd
2O
3, Sm
2O
3, Mn
2O
3, Co
2O
3, Pr
2O
3Powder or corresponding carbonate and nitrate powder are as raw material, according to Bi
1-xA
xFe
1-yB
yO
3(0≤x＜0.5,0≤y＜0.2, A is rare earth ion La
3+, Nd
3+, Td
3+, Sm
3+, Pr
3+In one or both, B is a kind of trivalent metal ion Mn
3+Or Co
3+Concrete composition sees Table two) the stoicheiometry batching of series ceramic.
B) even the powder mixes of batching, the average grain of mixture is less than 1.0 microns.
C) make water etc. easily evaporable liquid as tackiness agent mixture and tackiness agent are mixed, press target again.The thickness of target is 0.5mm.It is thick to reduce target, helps that heat is transmitted to target center fast in the sintering process from the surface, helps improving the heat-up rate of target center.
D) use vacuum or antivacuum baking oven, allowing the tackiness agent in the mixture volatilize fully totally below 400 ℃.Use easy evaporable tackiness agent, and before the sintering that is rapidly heated, remove tackiness agent, the volatilization that is tackiness agent in the sintering process absorbs heat, thus the heat-up rate when reducing sintering, to such an extent as to can not satisfy intensification condition more than the 30 ℃/s (degree/second).
E) use rapid thermal process RTA, tube furnace or other stove sintered ceramic, the heat-up rate above with 30 ℃/s (degree/second) heats up, and (is higher than Bi at 820 ℃
2O
3817 ℃ of fusing points) sintering Bi between 940 ℃
1-xA
xFe
1-yB
yO
3Series ceramic, sintering time be last fast cooling between 1 minute to 1 hour.Pottery behind the sintering becomes ABO
3Single-phase, resistivity can reach～and 10
9Ω cm and breakdown electric field are greater than 150kV/cm.
If the bigger target that preparation PLD or magnetron sputtering etc. use.The further prioritization scheme of the inventive method is: based on the above method, increase following steps:
F) previous step is prepared successful target grind into powder again, in powder, add suitable quantity of water, mix, prepare big target then again.Big target was put into 100 ℃～400 ℃ baking oven insulation more than 12 hours, allowed water fully volatilize, and relief target is warming up to more than 800 ℃ with the speed more than the 50 ℃/s (degree/second), and in being incubated 60 minutes under this temperature.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Table 1, other people Bi of having prepared at present
1-xA
xFe
1-yB
yO
3Stupalith and residual polarization thereof and voltage breakdown
The concrete preparation method of magneto-electric coupled ceramic materials of the present invention:
A) utilize Bi
2O
3, La
2O
3, Fe
2O
3, Td
2O
3, Nd
2O
3, Sm
2O
3, Mn
2O
3, Co
2O
3, Pr
2O
3Powder or corresponding carbonate and nitrate powder are as raw material, according to Bi
1-xA
xFe
1-yB
yO
3(0≤x＜0.5,0≤y＜0.2, A is rare earth cation La
3+, Nd
3+, Td
3+, Sm
3+, Pr
3+In one or both, B is transition metal ion Mn
3+, Co
3+In a kind of, concrete composition sees Table two) the stoicheiometry batching of series ceramic.
B) after the batching, powder is put into the agate jar grind more than 12 hours, allow the powder uniform mixing, and the average grain of powder is less than 1.0 microns.
C), add just an amount of water then as tackiness agent the powder oven dry that mixes.Mixture is pressed into target, and the thickness of target is 0.5mm.It is thick to reduce target, helps that heat is transmitted to target center fast in the sintering process from the surface, helps improving the heat-up rate of target center.
D) regulate temperature of oven to 150 ℃, target was incubated in baking oven more than 10 hours, and purpose is to allow the steam that contains in the target fully volatilize.Making water as tackiness agent, and allowed its volatilization clean before sintering, is that the volatilization of water absorbs heat in the sintering process that is rapidly heated, thus heat-up rate when reducing sintering.
E) use rapid thermal process (RTA), the heat-up rate above with 30 ℃/s (degree/second) heats up, and (is higher than Bi at 820 ℃
2O
3817 ℃ of fusing points) sintering Bi between 940 ℃
1-xA
xFe
1-yB
yO
3Series ceramic, sintering time is between 1 minute to 1 hour.Such as sintering BiFeO
3Sample, was cooled to below 500 degree with interior at 5 minutes again 870 ℃ of insulations 5 minutes with interior 870 degree that are warming up in 30 seconds then.Pottery behind the sintering becomes ABO
3Single-phase, resistivity can reach-10
9Ω cm and breakdown electric field are greater than 150kV/cm.
F) if the bigger target that preparation PLD or magnetron sputtering etc. use.The target of previous step sintering success grind into powder again, add entry as tackiness agent, be pressed into big target again, in baking oven, allow water fully volatilize then, in sintering more than 817 ℃ 1 hour.Such as BiFeO
3Sample is warming up to 830 ℃ and be incubated 10 minutes with the above speed of 50 ℃/s (degree/second).
The contriver sees Table 2 by the magneto-electric coupled ceramic materials and the physicals test result thereof of the preparation of foregoing invention method.
Table 2
Claims (5)
1, a kind of magneto-electric coupled ceramic materials is characterized in that:
(1) chemical formula is
Bi
1-xA
xFe
1-yB
yO
3
Wherein: 0≤x＜0.5,0≤y＜0.2 and x, y can not be 0 simultaneously;
A is one or both among rare earth cation La, Nd, Td, Sm, the Pr;
B is transition metal ion Mn or Co;
(2) has following physicals
Breakdown electric field is greater than 150kV/cm, and the residual polarization of electropolarization-electric field loop line is at 3～30 μ C/cm
2Between.
2, magneto-electric coupled ceramic materials according to claim 1 is characterized in that: described stupalith makes with following method:
When sintering, the heat-up rate above with 30 ° of degree/seconds heats up sintering, fast cooling then between 850 ℃ to 940 ℃.
3, magneto-electric coupled ceramic materials according to claim 1 is characterized in that: described stupalith makes with following method:
A) utilize Bi
2O
3, La
2O
3, Fe
2O
3, Td
2O
3, Nd
2O
3, Sm
2O
3, Mn
2O
3, Co
2O
3, Pr
2O
3Powder or corresponding carbonate and nitrate powder are as raw material, according to Bi
1-xA
xFe
1-yB
yO
3The stoicheiometry batching of pottery;
B) even the powder mixes of batching, the average grain of mixture is less than 1.0 microns;
C) make water etc. easily evaporable liquid as tackiness agent mixture and tackiness agent are mixed, press target again;
D) in the tackiness agent volatilization that allows below 400 ℃ in the mixture;
E) with 30 degree/seconds above heat-up rate heat up, sintering between 850 ℃ to 940 ℃, sintering time between 1 minute to 1 hour, last fast cooling.
4, the preparation method of a kind of claim 1,2 or 3 described magneto-electric coupled ceramic materials the steps include:
A) utilize Bi
2O
3, La
2O
3, Fe
2O
3, Td
2O
3, Nd
2O
3, Sm
2O
3, Mn
2O
3, Co
2O
3, Pr
2O
3Powder or corresponding carbonate and nitrate powder are as raw material, according to Bi
1-xA
xFe
1-yB
yO
3The stoicheiometry batching of pottery;
B) even the powder mixes of batching, the average grain of mixture is less than 1.0 microns;
C) make water etc. easily evaporable liquid as tackiness agent mixture and tackiness agent are mixed, press target again;
D) in the tackiness agent volatilization that allows below 400 ℃ in the mixture;
E) with 30 degree/seconds above heat-up rate heat up, sintering between 850 ℃ to 940 ℃, sintering time between 1 minute to 1 hour, last fast cooling.
5, the preparation method of magneto-electric coupled ceramic materials according to claim 4 is characterized in that:
F) the successful target grind into powder of previous step preparation, average grain is less than 1.0 microns; Make water etc. easily evaporable liquid as tackiness agent mixture and tackiness agent are mixed, prepare big target again; The target temperature is remained on 100 ℃～400 ℃, allow tackiness agent volatilization in the mixture; The heat-up rate above with 50 degree/seconds heats up, sintering between 800 ℃ to 940 ℃, sintering time between 1 minute to 1 hour, last fast cooling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410064900.9A CN1272277C (en) | 2004-10-10 | 2004-10-10 | Magneto-electric coupled ceramic materials and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410064900.9A CN1272277C (en) | 2004-10-10 | 2004-10-10 | Magneto-electric coupled ceramic materials and preparing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1603279A true CN1603279A (en) | 2005-04-06 |
| CN1272277C CN1272277C (en) | 2006-08-30 |
Family
ID=34666428
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044628A (en) * | 2008-04-01 | 2011-05-04 | 精工爱普生株式会社 | Piezoelectric material and piezoelectric element |
| CN102633443A (en) * | 2012-02-27 | 2012-08-15 | 陕西科技大学 | Method for preparing Tb-doped BiFeO3 ferroelectric film on surface of conductive glass substrate |
| CN103343315A (en) * | 2013-06-04 | 2013-10-09 | 南京理工大学 | Bismuth-ferrite-doped semiconductor film material and preparation method thereof |
| CN109516796A (en) * | 2018-11-30 | 2019-03-26 | 江西科技学院 | A kind of multiferroic solid solution ceramic and preparation method thereof |
| CN111205078A (en) * | 2020-01-13 | 2020-05-29 | 桂林电子科技大学 | Bi1-xNdxFeO3Preparation method of rare earth ferrite magnetic wave-absorbing material |
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2004
- 2004-10-10 CN CN200410064900.9A patent/CN1272277C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044628A (en) * | 2008-04-01 | 2011-05-04 | 精工爱普生株式会社 | Piezoelectric material and piezoelectric element |
| CN102044628B (en) * | 2008-04-01 | 2014-03-12 | 精工爱普生株式会社 | Piezoelectric material and piezoelectric element |
| CN102633443A (en) * | 2012-02-27 | 2012-08-15 | 陕西科技大学 | Method for preparing Tb-doped BiFeO3 ferroelectric film on surface of conductive glass substrate |
| CN103343315A (en) * | 2013-06-04 | 2013-10-09 | 南京理工大学 | Bismuth-ferrite-doped semiconductor film material and preparation method thereof |
| CN103343315B (en) * | 2013-06-04 | 2016-07-06 | 南京理工大学 | A kind of doped bismuth ferrite semiconductor film material and preparation method thereof |
| CN109516796A (en) * | 2018-11-30 | 2019-03-26 | 江西科技学院 | A kind of multiferroic solid solution ceramic and preparation method thereof |
| CN109516796B (en) * | 2018-11-30 | 2021-07-09 | 江西科技学院 | Multiferroic solid solution ceramic and preparation method thereof |
| CN111205078A (en) * | 2020-01-13 | 2020-05-29 | 桂林电子科技大学 | Bi1-xNdxFeO3Preparation method of rare earth ferrite magnetic wave-absorbing material |
| 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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| Publication number | Publication date |
|---|---|
| CN1272277C (en) | 2006-08-30 |
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