CN102898132B - 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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CN102898132B
CN102898132B CN201210397951.8A CN201210397951A CN102898132B CN 102898132 B CN102898132 B CN 102898132B CN 201210397951 A CN201210397951 A CN 201210397951A CN 102898132 B CN102898132 B CN 102898132B
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dielectric constant
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preparation
mixed powder
composite material
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CN102898132A (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, along with the high speed development of information, communication and Internet technology, require the transmission of high-speed data and high current density, electronic circuit is day by day to microminiaturized, integrated future development, and this has just proposed the requirement of miniaturization, lightweight and multifunction to electron device, complete machine and system.Therefore, the microminiaturization of the components and parts including electrical condenser and miniaturization are inexorable trends.And the larger material of effective dielectric constant takies identical resource and can obtain larger electric capacity, thereby meet the function on various circuit.Because huge dielectric constant material just can use resource still less, take volume still less.Therefore, research and develop efficient huge dielectric constant material and have very important meaning for the development of large-scale integrated circuit technology.Ferroelectric/ferromagnetic composite material has electric capacity and inductance two specific characters concurrently, can be the integrated more more options that provide of electric capacity, inductive part in electron device, can meet again the miniaturization of device and integrated.Meanwhile, LTCC (LTCC) technology becomes the main way of current passive integration gradually with its excellent electronics, thermomechanical and the characteristic such as interconnected.Ferroelectric/ferromagnetic composite material is combined with LTCC technology that not only to contribute to solve current LTCC material category single, performance does not realize the problem of seriation, can also realize with single-material the function of electric capacity and inductive part simultaneously, thus not mating of may occurring while avoiding capacitor layers and inductor layer material to burn altogether.But the overwhelming majority has the sintering temperature of huge dielectric constant magnetic electric compound material up to 1300 DEG C of left and right, cannot reach 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, magnetic permeability when 1 megahertz is 8 ~ 55.
Preparation method of the present invention, comprises the following steps:
1) by analytically pure Bi 2o 3and TiO 2press chemical general formula Bi 4ti 3o 12ball milling after preparation, dries, and sieves, and briquetting, through 840 ~ 860 DEG C of pre-burnings 4 ~ 6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 preparation, dries, and sieves, and briquetting, through 800 ~ 820 DEG C of pre-burnings 4 ~ 6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain Ni 0.37cu 0.20zn 0.43fe 1.92o 3.88powder;
3) by 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 obtain mixed powder, and wherein x is Bi 4ti 3o 12mass percent, and 0.2≤x≤0.6;
4) to the PVA tackiness agent granulation that adds mixed powder mass fraction 8%～15% in mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
5) by the compression moulding on demand of the mixed powder of matrix material, at 550 DEG C, be incubated 4 hours and get rid of binder PVA, within 2 ~ 4 hours, become porcelain at 940 ~ 950 DEG C of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
Described PVA tackiness agent adopts the polyvinyl alcohol water solution that mass fraction is 5%.
Object preparation method's sintering temperature of the present invention is low, and sintering temperature is 950 DEG C, has huge dielectric constant, and 20 hertz time, specific inductivity is up to 13000 ~ 65000, and magnetic permeability is higher, and magnetic permeability when 1 megahertz is 8 ~ 55.
Brief description of the 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 DEG C, 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 DEG C, 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 DEG C, 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 DEG C, is incubated the frequently figure of Jie of the matrix material of preparation in 4 hours.
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 DEG C, is incubated the frequently figure of Jie of the matrix material of preparation in 3 hours.
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 DEG C, is incubated the frequently figure of Jie of the matrix material of preparation in 2 hours.
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 DEG C,, 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 DEG C, 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 DEG C, 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) by analytically pure Bi 2o 3and TiO 2press chemical general formula Bi 4ti 3o 12ball milling after preparation, dries, and sieves, and briquetting, through 840 DEG C of pre-burnings 6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 preparation, dries, and sieves, and briquetting, through 820 DEG C of pre-burnings 4 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 obtain mixed powder;
4) to the PVA tackiness agent granulation that adds mixed powder mass fraction 8% in mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent adopts the polyvinyl alcohol water solution that mass fraction is 5%;
5) by the compression moulding on demand of the mixed powder of matrix material, at 550 DEG C, be incubated 4 hours and get rid of binder PVA, within 4 hours, become porcelain at 940 DEG C of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 1, in the matrix material that prepared by the present embodiment, only contain Bi 4ti 3o 12and Ni 0.37cu 0.20zn 0.43fe 1.92o 3.88two-phase, exists without other dephasign.
As seen from Figure 4, matrix material prepared by the present embodiment has huge dielectric constant effect, and 20 hertz time, specific inductivity is 32500.
As seen from Figure 7, matrix material prepared by the present embodiment has good magnetic, and magnetic permeability when 1 megahertz is 55.
Embodiment 2:
1) by analytically pure Bi 2o 3and TiO 2press chemical general formula Bi 4ti 3o 12ball milling after preparation, dries, and sieves, and briquetting, through 850 DEG C of pre-burnings 5 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 preparation, dries, and sieves, and briquetting, through 800 DEG C of pre-burnings 6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 obtain mixed powder;
4) to the PVA tackiness agent granulation that adds mixed powder mass fraction 12% in mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent adopts the polyvinyl alcohol water solution that mass fraction is 5%;
5) by the compression moulding on demand of the mixed powder of matrix material, at 550 DEG C, be incubated 4 hours and get rid of binder PVA, within 3 hours, become porcelain at 945 DEG C of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 2, in the matrix material that prepared by the present embodiment, only contain Bi 4ti 3o 12and Ni 0.37cu 0.20zn 0.43fe 1.92o 3.88two-phase, exists without other dephasign.
As seen from Figure 5, matrix material prepared by the present embodiment has huge dielectric constant effect, and 20 hertz time, specific inductivity is 65000.
As seen from Figure 8, matrix material prepared by the present embodiment has good magnetic, and magnetic permeability when 1 megahertz is 22.
Embodiment 3:
1) by analytically pure Bi 2o 3and TiO 2press chemical general formula Bi 4ti 3o 12ball milling after preparation, dries, and sieves, and briquetting, through 860 DEG C of pre-burnings 4 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 preparation, dries, and sieves, and briquetting, through 810 DEG C of pre-burnings 5 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 obtain mixed powder;
4) to the PVA tackiness agent granulation that adds mixed powder mass fraction 15% in mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
Described PVA tackiness agent adopts the polyvinyl alcohol water solution that mass fraction is 5%;
5) by the compression moulding on demand of the mixed powder of matrix material, at 550 DEG C, be incubated 4 hours and get rid of binder PVA, within 2 hours, become porcelain at 950 DEG C of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
As seen from Figure 3, in the matrix material that prepared by the present embodiment, only contain Bi 4ti 3o 12and Ni 0.37cu 0.20zn 0.43fe 1.92o 3.88two-phase, exists without other dephasign.
As seen from Figure 6, matrix material prepared by the present embodiment has huge dielectric constant effect, and 20 hertz time, specific inductivity is 13000.
As seen from Figure 9, matrix material prepared by the present embodiment has good magnetic, and magnetic permeability when 1 megahertz is 8.8.

Claims (3)

1. a low temperature co-fired magnetic electric compound material with huge dielectric constant, is characterized in that: the synthetic expression formula of 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, magnetic permeability when 1 megahertz is 8～55.
2. a preparation method for the low temperature co-fired magnetic electric compound material with huge dielectric constant as claimed in claim 1, is characterized in that comprising the following steps:
1) by analytically pure Bi 2o 3and TiO 2press chemical general formula Bi 4ti 3o 12ball milling after preparation, dries, and sieves, and briquetting, through 840～860 DEG C of pre-burnings 4～6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain 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 preparation, dries, and sieves, and briquetting, through 800～820 DEG C of pre-burnings 4～6 hours, crosses 120 mesh sieves after then gained bulk sample being pulverized and obtain Ni 0.37cu 0.20zn 0.43fe 1.92o 3.88powder;
3) by 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 obtain mixed powder, and wherein x is Bi 4ti 3o 12mass percent, and 0.2≤x≤0.6;
4) to the PVA tackiness agent granulation that adds mixed powder mass fraction 8%～15% in mixed powder, sieve through 60 orders and 120 eye mesh screens, obtain the mixed powder of required matrix material;
5) by the compression moulding on demand of the mixed powder of matrix material, at 550 DEG C, be incubated 4 hours and get rid of binder PVA, within 2～4 hours, become porcelain at 940～950 DEG C of sintering, obtain having the low temperature co-fired magnetic electric compound material of huge dielectric constant.
3. the preparation method of the low temperature co-fired magnetic electric compound material that has huge dielectric constant according to claim 2, is characterized in that: described PVA tackiness agent adopts the polyvinyl alcohol water solution that mass fraction is 5%.
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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TW201600489A (en) * 2014-06-30 2016-01-01 Walsin Technology Corp Low temperature heterogeneous co-fired magnetic dielectric ceramic composite material and preparation method thereof
CN104446449B (en) * 2014-11-26 2017-07-14 陕西科技大学 A kind of preparation method of BIT Fe multiferroic ferroelectric bulk ceramics
CN104987056B (en) * 2015-06-30 2018-01-12 电子科技大学 A kind of ferroelectric and ferromagnetic composite material and preparation method thereof
CN109279890B (en) * 2018-09-21 2021-05-14 歌尔光学科技有限公司 Preparation method of magnetoelectric composite 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

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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

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