CN102826842A - Multiferroic composite material with magneto-dielectric effect and preparation method thereof - Google Patents
Multiferroic composite material with magneto-dielectric effect and preparation method thereof Download PDFInfo
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- CN102826842A CN102826842A CN2012103499385A CN201210349938A CN102826842A CN 102826842 A CN102826842 A CN 102826842A CN 2012103499385 A CN2012103499385 A CN 2012103499385A CN 201210349938 A CN201210349938 A CN 201210349938A CN 102826842 A CN102826842 A CN 102826842A
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Abstract
The invention discloses a multiferroic composite ceramic material with a magneto-dielectric effect, the chemical formula of the material is NaNbO3-NiFe2O4, and the molar ratio is 1:1. The material is prepared by taking Na2CO3, Nb2O5, NiO and Fe2O3 as raw materials through adopting a solid phase method, carrying out material preparing and ball milling on the raw materials, burning an obtained object at a temperature of 900-1150 DEG C, carrying out compression moulding on the obtained object, and sintering the obtained object at a temperature of 1100-1200 DEG C. The multiferroic composite ceramic material disclosed by the invention has the advantages of good uniformity, small roughness, no micro-crack, stable performance, good electrical properties, magnetic properties, magneto-dielectric effect, and the like, and can be used for manufacturing integrated multifunctional magnetic/electrical parts; and the multiferroic composite ceramic material is simple in preparation process, non-toxic, small in pollution, and wide in application range.
Description
Technical field
The invention belongs to a kind of is the ceramic composition of characteristic with the composition, particularly a kind of unleaded many iron property particle composite ceramic material with magnetic dielectric coupling effect and preparation method thereof.
Background technology
Along with progress of science and technology, to miniaturization of devices, integrated require increasingly highly, therefore the novel material of development with two or more function has significant values.Multi-iron material since have simultaneously magnetic with electrically and intercouple, have in transmitter or transverter preparation field and to use widely and enjoy attention.The magnetic dielectric effect is the same with electronics ferroelectricity and magnetoelectric effect, is the important physical of multi-ferroic material.Magnetic dielectric effect MDE (Magneto-dielectric Effect) definition is: multi-ferroic material produces the sudden change of specific inductivity near Tc (ferromagnetic phase transition point), and the specific inductivity that perhaps below Tc, produces with changes of magnetic field changes.The sign formula of magnetic dielectric effect is:
MDE(%)=[ε(H)-ε(0)]/ε(0)×100%
Specific inductivity when ε (H) and ε (0) are respectively magnetic field and no magnetic field.The magnetic dielectric materials has all proposed series of new problems owing to relate to magnetics and electricity and both intersections to experiment and theoretical investigation.The magnetic dielectric materials had caused domestic and international expert's very big concern in recent years.
At present multi-iron material mainly is divided into single-phase compound multi-iron material and complex phase mixture multi-iron material, and relatively rareness and its Tc are low owing to have the single-phase many iron cpds of intrinsic, and the complex phase multi-iron material has caused extensive concern in recent years.First composite system BaTiO
3-CoFe
2O
4Be in the news in the seventies in 20th century, thereafter, a series of BaTiO
3, Pb (Zr
0.5Ti
0.5) O
3The composite material system is studied in succession.Has 4.54% magnetic dielectric effect (In " Effect of the piezomagnetic NiFe like the 0.15NFO-0.85PMN-PT matrix material of people such as ArifD Sheikh preparation
2O
4Phase on the piezoelectric Pb (Mg
1/3Nb
2/3)
0.67Ti
0.33O
3Phase in magnetoelectric composites ", Smart Mater.Struct., 2009,18:065014); People such as S.Y.Tan have obtained 0.5MgFe
2O
4-0.5BaTiO
3The magnetic dielectric effect of system under 7KOe magnetic field is 0.466% (In " Synthesis and characterization of composite MgFe
2O
4-BaTiO
3Multiferroic system ", J.Appl.Phys., 2008,103:094105).But these material systems contain toxic substance mostly, and environmental pollution is serious.Developing unleaded nontoxic new composite system has great importance.
Sodium columbate (NaNbO
3) show high spontaneous polarization, high-k and high tension electricity coefficient under the basic piezoelectric room temperature.In addition, spinel structure nickel ferrite (NiFe
2O
4) material is because of having high resistivity and high piezomagnetic coefficient is widely used in the exploitation of many iron property composite system.Many iron property composite ceramic material involved in the present invention is to propose first, does not see relevant report at present both at home and abroad.
Summary of the invention
The object of the invention provides a kind of unleaded, nontoxic novel many iron property composite system with good electric property, magnetic property and magnetic dielectric effect and preparation method thereof.The present invention is with Na
2CO
3, Nb
2O
5, NiO and Fe
2O
3Be raw material, adopt the solid phase method preparation to have many iron property composite ceramic material of magnetic dielectric effect.
The present invention is achieved through following technical scheme.
A kind of many iron property composite ceramic material with magnetic dielectric effect, its chemical formula is NaNbO
3-NiFe
2O
4, mol ratio is 1:1;
The preparation method of this composite ceramic material has following steps:
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4, mol ratio is that 1:1 prepares burden; With material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds and places the polyester jar, ball milling 4 ~ 24 hours;
(2), cross 40 mesh sieves with 100~120 ℃ of oven dry in loft drier of the raw material behind step (1) ball milling;
(3) powder after step (2) is dried, sieved is put into moderate oven, in 900~1150 ℃ of pre-burnings, is incubated 2 ~ 8 hours;
(4) powder after step (3) pre-burning being added mass percent is that 8% ~ 10% paraffin carries out granulation as tackiness agent, crosses 80 mesh sieves, suppresses green compact with powder compressing machine;
(5) with the green compact of step (4) in 1100 ℃~1200 ℃ sintering, be incubated 2 ~ 8 hours, make many iron property composite ceramic material.
The ball milling of said step (1) adopts planetary ball mill, and rotating speed is 1000 rev/mins.
The pressure of the powder compressing machine of said step (4) is 4 ~ 8MPa.
The sintering temperature that said step (4) adopts is 1150 ℃.
The soaking time of said step (5) is 4 hours.
Compound multi-iron material of the present invention has good uniformity, roughness is little, non-microcracked; Stable performance, and have advantages such as good electric property, magnetic property and magnetic dielectric effect, sintering temperature is 1100 ~ 1200 ℃; Magnetic permeability is 1 ~ 2 (1MHz) under the 1GHz; Specific inductivity is 48 ~ 52 (1MHz), the magnetic dielectric imitate coefficient be 8~12% (1MHz, 3000Gauss).Can be used for making integrated multi-function magnetic/electrical part, preparation technology is simple, and is nontoxic, pollutes for a short time, has wide application field.
Embodiment
The present invention is with Na
2CO
3(analytical pure), Nb
2O
5(analytical pure), NiO (analytical pure), Fe
2O
3(analytical pure) is initial feed, prepares the many iron property matrix material with magnetic dielectric effect through solid phase method, and specific embodiment is following:
Embodiment 1
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 4 hours on planetary ball mill, and drum's speed of rotation is 1000 rev/mins;
(2) raw material behind the ball milling is placed loft drier,, cross 40 mesh sieves then in 120 ℃ of oven dry;
(3) powder after will drying, sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 4 hours;
(4) to add the quality percentage composition be that 8% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, use powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and be 20mm, thickness is the green compact of 5mm;
(5) with green compact at 1100 ℃ of sintering, be incubated 4 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test resulting product, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 2
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 12 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling is placed loft drier,, cross 40 mesh sieves then in 100 ℃ of oven dry;
(3) powder after will drying, sieving is put into moderate oven, in 1150 ℃ of pre-burnings, is incubated 4 hours;
(4) to add the quality percentage composition be that 8% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, use powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and be 20mm, thickness is the green compact of 5mm;
(5) with green compact at 1100 ℃ of sintering, be incubated 8 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 3
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 24 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier, in 120 ℃ of oven dry, then crosses 40 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 1100 ℃ of pre-burnings, is incubated 6 hours;
(4) to add the quality percentage composition be that 8% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, use powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and be 20mm, thickness is the green compact of 5mm;
(5) with green compact at 1125 ℃ of sintering, be incubated 4 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 4
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 4 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier, in 110 ℃ of oven dry, then crosses 40 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 1100 ℃ of pre-burnings, is incubated 4 hours;
(4) to add the quality percentage composition be that 9% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, uses powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and is 20mm, thickness is the green compact of about 5mm;
(5) with green compact at 1150 ℃ of sintering, be incubated 6 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 5
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 6 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier in 120 ℃ of oven dry, then crosses 80 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 4 hours;
(4) to add the quality percentage composition be that 10% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, uses powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and is 20mm, thickness is the green compact of about 5mm;
(5) with green compact at 1175 ℃ of sintering, be incubated 6 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 6
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 6 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier in 120 ℃ of oven dry, then crosses 80 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 6 hours;
(4) to add the quality percentage composition be that 10% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, uses powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and is 20mm, thickness is the green compact of about 5mm;
(5) with green compact at 1200 ℃ of sintering, be incubated 4 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 7
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 6 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier in 120 ℃ of oven dry, then crosses 80 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 4 hours;
(4) to add the quality percentage composition be that 10% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, uses powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and is 20mm, thickness is the green compact of about 5mm;
(5) with green compact at 1200 ℃ of sintering, be incubated 6 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Embodiment 8
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4Prepare burden NaNbO
3And NiFe
2O
4Mol ratio be 1:1, the mixed powder of 14g is put into the polyester jar, with material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds in the polyester jar, and ball milling is 6 hours on planetary ball mill; Rotating speed is 1000 rev/mins;
(2) raw material behind the ball milling places loft drier in 120 ℃ of oven dry, then crosses 80 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 900 ℃ of pre-burnings, is incubated 8 hours;
(4) to add the quality percentage composition be that 10% paraffin wax binder is carried out granulation to the powder after the pre-burning, cross 80 mesh sieves after, uses powder compressing machine under the pressure of 4MPa, powder to be pressed into diameter and is 20mm, thickness is the green compact of about 5mm;
(5) with green compact at 1200 ℃ of sintering, be incubated 8 hours, make many iron property composite ceramic material with magnetic dielectric effect.
With the dielectric properties of goods through Agilent E4991 electric impedance analyzer, 4285LCR analyser and dependence test anchor clamps test gained sample, magnetic property and magnetic dielectric effect, concrete test result sees table 1 for details.
Table 1
Claims (5)
1. many iron property composite ceramic material with magnetic dielectric effect, its chemical formula is NaNbO
3-NiFe
2O
4, mol ratio is 1:1.
The preparation method of this composite ceramic material has following steps:
(1) with Na
2CO
3And Nb
2O
5, NiO and Fe
2O
3Press stoichiometric equation NaNbO
3And NiFe
2O
4, mol ratio is that 1:1 prepares burden; With material: deionized water: the mass ratio of zirconium ball is that the ratio of 1:1:1.5 adds and places the polyester jar, ball milling 4 ~ 24 hours;
(2), cross 40 mesh sieves with 100 ~ 120 ℃ of oven dry in loft drier of the raw material behind step (1) ball milling;
(3) powder after step (2) is dried, sieved is put into moderate oven, in 900 ~ 1150 ℃ of pre-burnings, is incubated 2 ~ 8 hours;
(4) powder after step (3) pre-burning being added mass percent is that 8% ~ 10% paraffin carries out granulation as tackiness agent, crosses 80 mesh sieves, suppresses green compact with powder compressing machine;
(5) with the green compact of step (4) in 1100 ℃ ~ 1200 ℃ sintering, be incubated 2 ~ 8 hours, make many iron property composite ceramic material.
2. according to the many iron property composite ceramic material with magnetic dielectric effect of claim 1, it is characterized in that the ball milling of said step (1) adopts planetary ball mill, rotating speed is 1000 rev/mins.
3. according to the many iron property composite ceramic material with magnetic dielectric effect of claim 1, it is characterized in that the pressure of the powder compressing machine of said step (4) is 4 ~ 8MPa.
4. according to the many iron property composite ceramic material with magnetic dielectric effect of claim 1, it is characterized in that the sintering temperature that said step (4) adopts is 1150 ℃.
5. according to the many iron property composite ceramic material with magnetic dielectric effect of claim 1, it is characterized in that the soaking time of said step (5) is 4 hours.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2848281A1 (en) * | 2013-09-16 | 2015-03-18 | BIOTRONIK SE & Co. KG | Electrode device for a medical implant, and medical implant comprising an electrode device |
CN107078376A (en) * | 2014-08-21 | 2017-08-18 | 罗杰斯公司 | Using magnetic dielectric material, with channel spacing from multi-input/output antenna |
CN112745115A (en) * | 2021-01-11 | 2021-05-04 | 电子科技大学 | Magnetostrictive material with high strain sensitivity in low magnetic field and preparation method thereof |
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CN102557635A (en) * | 2011-12-22 | 2012-07-11 | 四川师范大学 | Sodium niobate lithium tantalate series lead-free piezoelectric ceramic composite |
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2012
- 2012-09-18 CN CN2012103499385A patent/CN102826842A/en active Pending
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CN102557635A (en) * | 2011-12-22 | 2012-07-11 | 四川师范大学 | Sodium niobate lithium tantalate series lead-free piezoelectric ceramic composite |
Non-Patent Citations (1)
Title |
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YAN MA ET AL.: "Enhanced multiferroic characteristics in NaNbO3-modified BiFeO3 ceramics", 《JOURNAL OF APPLIED PHYSICS》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2848281A1 (en) * | 2013-09-16 | 2015-03-18 | BIOTRONIK SE & Co. KG | Electrode device for a medical implant, and medical implant comprising an electrode device |
US9468756B2 (en) | 2013-09-16 | 2016-10-18 | Biotronik Se & Co. Kg | Electrode device for a medical implant, and a medical implant comprising an electrode device |
CN107078376A (en) * | 2014-08-21 | 2017-08-18 | 罗杰斯公司 | Using magnetic dielectric material, with channel spacing from multi-input/output antenna |
CN112745115A (en) * | 2021-01-11 | 2021-05-04 | 电子科技大学 | Magnetostrictive material with high strain sensitivity in low magnetic field and preparation method thereof |
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