CN102898132A - Low-temperature cofiring magnetoelectric composite material with giant dielectric constant and preparation method thereof - Google Patents

Low-temperature cofiring magnetoelectric composite material with giant dielectric constant and preparation method thereof Download PDF

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CN102898132A
CN102898132A CN2012103979518A CN201210397951A CN102898132A CN 102898132 A CN102898132 A CN 102898132A CN 2012103979518 A CN2012103979518 A CN 2012103979518A CN 201210397951 A CN201210397951 A CN 201210397951A CN 102898132 A CN102898132 A CN 102898132A
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dielectric constant
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mixed powder
composite material
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CN102898132B (en
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杨海波
杨艳艳
林营
朱建锋
王芬
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a low-temperature cofiring magnetoelectric composite material with a giant dielectric constant and a preparation method thereof. The low-temperature cofiring magnetoelectric composite material with the giant dielectric constant comprises the following steps of: mixing and carrying out ball milling to Bi2O3 and TiO2, drying, screening, briquetting, pre-sintering, smashing, and screening by a sieve of 120 meshes to obtain Bi4Ti3O12 powder; after mixing NiO, CuO, ZnO and Fe2O3, carrying out ball milling, drying, screening, briquetting, pre-sintering, smashing, and screening by a sieve of 120 meshes to obtain Ni0.37Cu0.20Zn0.43Fe1.92O3.88powder; evenly mixing the Bi4Ti3O12 powder with the Ni0.37Cu0.20Zn0.43Fe1.92O3.88powder to obtain mixed powder; adding PVA (polyvinyl alcohol) adhesive into the mixed powder for granulation; screening by sieves of 60 and 120 meshes to obtain the mixed powder of the required composite material; pressing and forming the mixed powder of the composite material according to the requirement; removing the adhesive PVA; and sintering to obtain porcelain at the temperature of 940-950DEG C so as to obtain the low-temperature cofiring magnetoelectric composite material with the giant dielectric constant, wherein the dielectric constant of the composite material is 13000-65000 at 20Hz, and the magnetic conductivity of the composite material is 8-55 at 1MHz.

Description

A kind of low temperature co-fired magnetic electric compound material with huge dielectric constant and preparation method thereof
Technical field
The invention belongs to material science, relate to a kind of low temperature co-fired magnetic electric compound material with huge dielectric constant and preparation method thereof.
Background technology
In recent years, high speed development along with information, communication and Internet technology, require the transmission of high-speed data and high current density, to microminiaturized, integrated future development, this has just proposed the requirement of miniaturization, lightweight and multifunction to electronic circuit to electron device, complete machine and system day by day.Therefore, the microminiaturization and the miniaturization that comprise the components and parts of electrical condenser are inexorable trends.And the larger material of effective dielectric constant takies identical resource and can obtain larger electric capacity, thereby satisfies the function on the various circuit.Because the huge dielectric constant material just can use resource still less, takies volume still less.Therefore, research and develop out efficient huge dielectric constant material and for the development of large-scale integrated circuit technology very important meaning is arranged.Ferroelectric/ferromagnetic composite material has electric capacity and inductance two specific characters concurrently, and the integrated more more options that provide of electric capacity, inductive part in the electron device can be provided, can satisfy again the miniaturization of device and integrated.Meanwhile, LTCC (LTCC) technology becomes the main way of present passive integration gradually with its excellent electronics, heat engine tool and the characteristic such as interconnected.Ferroelectric/ferromagnetic composite material is combined with the LTCC technology that not only to help to solve present LTCC material category single, performance does not realize the problem of seriation, can also realize simultaneously with single-material the function of electric capacity and inductive part, thus not mating of may occurring when avoiding capacitor layers and inductor layer material to burn altogether.Yet, the sintering temperature that the overwhelming majority has a huge dielectric constant magnetic electric compound material up to 1300 ℃ about, can't reach the LTCC technical requirements.
Summary of the invention
The object of the present invention is to provide a kind of sintering temperature low, preparation technology simply has low temperature co-fired magnetic electric compound material of huge dielectric constant and preparation method thereof.
For achieving the above object, the synthetic expression formula of reaction that the present invention has the low temperature co-fired magnetic electric compound material of huge dielectric constant is xBi 4Ti 3O 12/ (1-x) Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88, wherein x is Bi 4Ti 3O 12Mass percent, and 0.2≤x≤0.6, specific inductivity is up to 13000 ~ 65000 in the time of 20 hertz for this matrix material, the magnetic permeability during 1 megahertz is 8 ~ 55.
Preparation method of the present invention may further comprise the steps:
1) with analytically pure Bi 2O 3And TiO 2Press chemical general formula Bi 4Ti 3O 12Ball milling after the preparation, oven dry is sieved, and briquetting through 840 ~ 860 ℃ of pre-burnings 4 ~ 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Bi 4Ti 3O 12Powder;
2) analytically pure NiO, CuO, ZnO and Fe 2O 3Press chemical general formula Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Ball milling after the preparation, oven dry is sieved, and briquetting through 800 ~ 820 ℃ of pre-burnings 4 ~ 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder;
3) with Bi 4Ti 3O 12Powder and Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder is pressed xBi 4Ti 3O 12/ (1-x) Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Expression formula mixes to get mixed powder, and wherein x is Bi 4Ti 3O 12Mass percent, and 0.2≤x≤0.6;
4) add the PVA tackiness agent granulation of mixed powder mass fraction 8%~15% in the mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
5) with the on demand compression moulding of mixed powder of matrix material, at 550 ℃, be incubated 4 hours and get rid of binder PVA, became porcelain in 2 ~ 4 hours at 940 ~ 950 ℃ of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
Described PVA tackiness agent employing mass fraction is 5% polyvinyl alcohol water solution.
Purpose preparation method's sintering temperature of the present invention is low, and sintering temperature is 950 ℃, has huge dielectric constant, and specific inductivity is up to 13000 ~ 65000 in the time of 20 hertz, and magnetic permeability is higher, and the magnetic permeability during 1 megahertz is 8 ~ 55.
Description of drawings
Fig. 1 is for working as Bi 4Ti 3O 12Mass ratio be 20%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 80%, sintering temperature is 940 ℃, is incubated the XRD figure of matrix material of preparation in 4 hours.
Fig. 2 is for working as Bi 4Ti 3O 12Mass ratio be 40%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 60%, sintering temperature is 945 ℃, is incubated the XRD figure of matrix material of preparation in 3 hours.
Fig. 3 is for working as Bi 4Ti 3O 12Mass ratio be 60%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 40%, sintering temperature is 950 ℃, is incubated the XRD figure of matrix material of preparation in 2 hours.
Fig. 4 is for working as Bi 4Ti 3O 12Mass ratio be 20%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 80%, sintering temperature is 940 ℃, Jie of matrix material who is incubated preparation in 4 hours schemes frequently.
Fig. 5 is for working as Bi 4Ti 3O 12Mass ratio be 40%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 60%, sintering temperature is 945 ℃, Jie of matrix material who is incubated preparation in 3 hours schemes frequently.
Fig. 6 is for working as Bi 4Ti 3O 12Mass ratio be 60%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 40%, sintering temperature is 950 ℃, Jie of matrix material who is incubated preparation in 2 hours schemes frequently.
Fig. 7 is for working as Bi 4Ti 3O 12Mass ratio be 20%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 80%, sintering temperature is 940 ℃,, be incubated the magnetic property of matrix material of preparation in 4 hours.
Fig. 8 is for working as Bi 4Ti 3O 12Mass ratio be 40%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 60%, sintering temperature is 945 ℃, is incubated the magnetic property of matrix material of preparation in 3 hours.
Fig. 9 is for working as Bi 4Ti 3O 12Mass ratio be 60%, Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Mass ratio be 40%, sintering temperature is 950 ℃, is incubated the magnetic property of matrix material of preparation in 2 hours.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:
1) with analytically pure Bi 2O 3And TiO 2Press chemical general formula Bi 4Ti 3O 12Ball milling after the preparation, oven dry is sieved, and briquetting through 840 ℃ of pre-burnings 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Bi 4Ti 3O 12Powder;
2) analytically pure NiO, CuO, ZnO and Fe 2O 3Press chemical general formula Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Ball milling after the preparation, oven dry is sieved, and briquetting through 820 ℃ of pre-burnings 4 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder;
3) get by mass percentage 20% Bi 4Ti 3O 12Powder and 80% Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder mixes to get mixed powder;
4) add the PVA tackiness agent granulation of mixed powder mass fraction 8% in the mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent employing mass fraction is 5% polyvinyl alcohol water solution;
5) with the on demand compression moulding of mixed powder of matrix material, at 550 ℃, be incubated 4 hours and get rid of binder PVA, became porcelain in 4 hours at 940 ℃ of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 1, only contain Bi in the matrix material of the present embodiment preparation 4Ti 3O 12And Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Two-phase exists without other dephasign.
As seen from Figure 4, the matrix material of the present embodiment preparation has the huge dielectric constant effect, and specific inductivity is 32500 in the time of 20 hertz.
As seen from Figure 7, the matrix material of the present embodiment preparation has preferably magnetic, and the magnetic permeability during 1 megahertz is 55.
Embodiment 2:
1) with analytically pure Bi 2O 3And TiO 2Press chemical general formula Bi 4Ti 3O 12Ball milling after the preparation, oven dry is sieved, and briquetting through 850 ℃ of pre-burnings 5 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Bi 4Ti 3O 12Powder;
2) analytically pure NiO, CuO, ZnO and Fe 2O 3Press chemical general formula Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Ball milling after the preparation, oven dry is sieved, and briquetting through 800 ℃ of pre-burnings 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder;
3) get by mass percentage 40% Bi 4Ti 3O 12Powder and 60% Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder mixes to get mixed powder;
4) add the PVA tackiness agent granulation of mixed powder mass fraction 12% in the mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent employing mass fraction is 5% polyvinyl alcohol water solution;
5) with the on demand compression moulding of mixed powder of matrix material, at 550 ℃, be incubated 4 hours and get rid of binder PVA, became porcelain in 3 hours at 945 ℃ of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 2, only contain Bi in the matrix material of the present embodiment preparation 4Ti 3O 12And Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Two-phase exists without other dephasign.
As seen from Figure 5, the matrix material of the present embodiment preparation has the huge dielectric constant effect, and specific inductivity is 65000 in the time of 20 hertz.
As seen from Figure 8, the matrix material of the present embodiment preparation has preferably magnetic, and the magnetic permeability during 1 megahertz is 22.
Embodiment 3:
1) with analytically pure Bi 2O 3And TiO 2Press chemical general formula Bi 4Ti 3O 12Ball milling after the preparation, oven dry is sieved, and briquetting through 860 ℃ of pre-burnings 4 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Bi 4Ti 3O 12Powder;
2) analytically pure NiO, CuO, ZnO and Fe 2O 3Press chemical general formula Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Ball milling after the preparation, oven dry is sieved, and briquetting through 810 ℃ of pre-burnings 5 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder;
3) get by mass percentage 60% Bi 4Ti 3O 12Powder and 40% Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder mixes to get mixed powder;
4) add the PVA tackiness agent granulation of mixed powder mass fraction 15% in the mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent employing mass fraction is 5% polyvinyl alcohol water solution;
5) with the on demand compression moulding of mixed powder of matrix material, at 550 ℃, be incubated 4 hours and get rid of binder PVA, became porcelain in 2 hours at 950 ℃ of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 3, only contain Bi in the matrix material of the present embodiment preparation 4Ti 3O 12And Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Two-phase exists without other dephasign.
As seen from Figure 6, the matrix material of the present embodiment preparation has the huge dielectric constant effect, and specific inductivity is 13000 in the time of 20 hertz.
As seen from Figure 9, the matrix material of the present embodiment preparation has preferably magnetic, and the magnetic permeability during 1 megahertz is 8.8.

Claims (3)

1. low temperature co-fired magnetic electric compound material with huge dielectric constant is characterized in that: the synthetic expression formula of the reaction of this matrix material is xBi 4Ti 3O 12/ (1-x) Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88, wherein x is Bi 4Ti 3O 12Mass percent, and 0.2≤x≤0.6, specific inductivity is up to 13000 ~ 65000 in the time of 20 hertz for this matrix material, the magnetic permeability during 1 megahertz is 8 ~ 55.
2. preparation method with low temperature co-fired magnetic electric compound material of huge dielectric constant is characterized in that may further comprise the steps:
1) with analytically pure Bi 2O 3And TiO 2Press chemical general formula Bi 4Ti 3O 12Ball milling after the preparation, oven dry is sieved, and briquetting through 840 ~ 860 ℃ of pre-burnings 4 ~ 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Bi 4Ti 3O 12Powder;
2) analytically pure NiO, CuO, ZnO and Fe 2O 3Press chemical general formula Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Ball milling after the preparation, oven dry is sieved, and briquetting through 800 ~ 820 ℃ of pre-burnings 4 ~ 6 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder;
3) with Bi 4Ti 3O 12Powder and Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Powder is pressed xBi 4Ti 3O 12/ (1-x) Ni 0.37Cu 0.20Zn 0.43Fe 1.92O 3.88Expression formula mixes to get mixed powder, and wherein x is Bi 4Ti 3O 12Mass percent, and 0.2≤x≤0.6;
4) add the PVA tackiness agent granulation of mixed powder mass fraction 8%~15% in the mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
5) with the on demand compression moulding of mixed powder of matrix material, at 550 ℃, be incubated 4 hours and get rid of binder PVA, became porcelain in 2 ~ 4 hours at 940 ~ 950 ℃ of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
3. the preparation method that the low temperature co-fired magnetic electric compound material of huge dielectric constant is arranged according to claim 2 is characterized in that: it is 5% polyvinyl alcohol water solution that described PVA tackiness agent adopts mass fraction.
CN201210397951.8A 2012-10-18 2012-10-18 Low-temperature cofiring magnetoelectric composite material with giant dielectric constant and preparation method thereof Expired - Fee Related CN102898132B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446449A (en) * 2014-11-26 2015-03-25 陕西科技大学 Preparation method of BIT-Fe multiferroic ferroelectric ceramic
CN104987056A (en) * 2015-06-30 2015-10-21 电子科技大学 Novel ferroelectric-ferromagnetic composite material and preparation method thereof
TWI562973B (en) * 2014-06-30 2016-12-21
CN109279890A (en) * 2018-09-21 2019-01-29 歌尔股份有限公司 The preparation method of magnetic electric compound material

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CN101792319A (en) * 2010-04-07 2010-08-04 陕西科技大学 Preparation method of low temperature sintered magnetoelectric composite ceramic material

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN101792319A (en) * 2010-04-07 2010-08-04 陕西科技大学 Preparation method of low temperature sintered magnetoelectric composite ceramic material

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Title
石敏等: "磁电复合材料的研究现状及发展趋势", 《金属功能材料》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI562973B (en) * 2014-06-30 2016-12-21
CN104446449A (en) * 2014-11-26 2015-03-25 陕西科技大学 Preparation method of BIT-Fe multiferroic ferroelectric ceramic
CN104987056A (en) * 2015-06-30 2015-10-21 电子科技大学 Novel ferroelectric-ferromagnetic composite material and preparation method thereof
CN109279890A (en) * 2018-09-21 2019-01-29 歌尔股份有限公司 The preparation method of magnetic electric compound material

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