CN104557028A - Layered magnetoelectric composite material and preparation method thereof - Google Patents
Layered magnetoelectric composite material and preparation method thereof Download PDFInfo
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- CN104557028A CN104557028A CN201510019033.5A CN201510019033A CN104557028A CN 104557028 A CN104557028 A CN 104557028A CN 201510019033 A CN201510019033 A CN 201510019033A CN 104557028 A CN104557028 A CN 104557028A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 124
- 230000004888 barrier function Effects 0.000 claims abstract description 23
- 238000000748 compression moulding Methods 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims description 59
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 48
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 48
- 239000003795 chemical substances by application Substances 0.000 claims description 41
- 239000000126 substance Substances 0.000 claims description 36
- 150000001875 compounds Chemical class 0.000 claims description 31
- 238000005469 granulation Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 5
- 238000005245 sintering Methods 0.000 abstract description 26
- 230000005621 ferroelectricity Effects 0.000 abstract description 9
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000005307 ferromagnetism Effects 0.000 abstract description 2
- 229910010252 TiO3 Inorganic materials 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 21
- 230000005291 magnetic effect Effects 0.000 description 20
- 239000000463 material Substances 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- 238000000227 grinding Methods 0.000 description 12
- 238000009792 diffusion process Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 230000005415 magnetization Effects 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 239000007775 ferroic material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910003321 CoFe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
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Abstract
The invention discloses a layered magnetoelectric composite material and a preparation method thereof. The preparation method comprises the following steps: granulating 0.65BaTiO3-0.35(Na0.5Bi0.5)TiO3 powder and BiY2Fe5O12 powder respectively, then carrying out compression moulding in a mould in a manner of 2-2 composite barrier layer superposition arrangement, then removing a PVA adhesive, and sintering at 1100-1150 DEG C to obtain the layered magnetoelectric composite material. According to the layered magnetoelectric composite material and the preparation method thereof disclosed by the invention, because the 0.65BaTiO3-0.35(Na0.5Bi0.5)TiO3 powder and the BiY2Fe5O12 powder are moulded in the manner of 2-2 composite barrier layer superposition arrangement to co-sinter a ferroelectric phase and a ferromagnetic phase in a layered composite manner, inter-reaction between the two phases can be effectively suppressed, thus keeping the respective characteristics, and enabling the layered magnetoelectric composite material to be good in both ferroelectricity and ferromagnetism.
Description
Technical field
The invention belongs to material science, relate to a kind of layered electromagnetic matrix material and preparation method thereof.
Background technology
Along with the development of information technology, the miniaturization of device, multifunction, make people constantly surging to the multifunctional material research interest such as electrical collector and magnetic.Therefore, the microminiaturization and the miniaturization that comprise the components and parts of ferroelectric dielectric materials and magneticsubstance are inexorable trends, and the magnetic electric compound material integrating ferroelectricity and ferromagnetism has identical volume can have more function on circuit.
Multi-ferroic material not only possesses various single ferrous (as ferroelectricity, ferromegnetism and ferroelasticity), and some new functions can be produced by the coupling synergy of ferrous, greatly widen the range of application of ferroic material, the components and parts utilizing multi-ferroic material to make have the functions such as conversion, transmission, process information, stored energy, save energy, are widely used in the field such as the energy, telecommunications, automatically control, communication, household electrical appliance, biology, health care, light industry, ore dressing, physics mine locating, military project.
Magnetic electric compound material is divided into 0-3 type magnetic electric compound material and 2-2 type magnetic electric compound material.0-3 type magnetic electric compound material be by discontinuous ferroelectric phase (ferromagnetic phase) Granular composite in the ferromagnetic phase (ferroelectric phase) of three-dimensional communication, mix according to a certain percentage, solid state sintering at a certain temperature, thus the particle magnetic electric compound material obtained.This kind of structure is simple, be study the earliest, a most widely used type.But because piezoelectric phase (ferromagnetic phase) exists the uneven problem of dispersion in ferromagnetic (piezoelectricity) matrix, thus the material magnetoelectric voltage coefficient of this kind of structure type is lower.2-2 type magnetic electric compound material makes it be total to the magnetic electric compound material together with burning with ferromagnetic phase powder according to the mode that barrier layer superposes ferroelectric phase powder.This kind of structure can adjust the content of pressure magnetic phase in a big way, so magnetoelectric voltage coefficient is greatly improved.Because ferroelectric phase layer that resistivity is very high can block the connection of Magnetic Phase layer completely, make the leakage current of material monolithic less, be conducive to the raising of material magnetic electricity performance.
Holland Philips laboratory is first the CoFe of ferromagnetic phase
2o
4with the BaTiO of ferroelectric phase
3powder mixes according to a certain percentage, and then heating up makes it congruent melting In-situ reaction, is finally cooled to the room temperature sosoloid that just to obtain with magnetoelectricity complex body be main component by certain speed.This method temperature is too high, easily produces some unpredictable phases, reduces the performance of matrix material.
Summary of the invention
The object of the present invention is to provide a kind of layered electromagnetic matrix material and preparation method thereof, ferroelectric-ferromagnetic is burnt together altogether in the mode of lamellar composite, effectively can suppress reacting to each other thus keeping respective characteristic between two-phase, make the layered electromagnetic matrix material of preparation not only have good ferroelectricity but also have good ferromegnetism.
For achieving the above object, the present invention adopts following technical scheme:
A kind of layered electromagnetic matrix material, the chemical formula of this layered electromagnetic matrix material is:
XBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.4.
The chemical formula of this layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.2.
The chemical formula of this layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.1.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3mixed by ball milling after preparation, then sieve, briquetting, then through 880 ~ 920 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3mixed by ball milling after preparation, then sieve, briquetting, then through 1000 ~ 1020 DEG C of pre-burnings 4 ~ 6 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder;
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.4, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound;
(5) at 1100 ~ 1150 DEG C, sinter 2 ~ 4 hours again after getting rid of PVA tackiness agent and become porcelain, obtain layered electromagnetic matrix material.
In described step (1), step (4), Ball-milling Time is 4 ~ 6 hours.
To 0.65BaTiO in described step (3)
3-0.35 (Na
0.5bi
0.5) TiO
3the quality adding PVA tackiness agent in powder is 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
38% ~ 15% of powder quality; To BiY
2fe
5o
12the quality adding PVA tackiness agent in powder is BiY
2fe
5o
128% ~ 15% of powder quality.
Described PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
The barrier layer of the middle 2-2 compound of described step (4) is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder, BiY
2fe
5o
12powder, 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder stacks together.
Described eliminating PVA tackiness agent is specifically: at temperature is 550-600 DEG C, be incubated 3-5 hour.
Compared with prior art, the beneficial effect that has of the present invention: the present invention is respectively by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder, BiY
2fe
5o
12after powder granulation, be arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound, then discharge PVA tackiness agent, sinter at 1100 ~ 1150 DEG C, layered electromagnetic matrix material can be obtained.Due to 0.65BaTiO in the present invention
3-0.35 (Na
0.5bi
0.5) TiO
3powder, BiY
2fe
5o
12powder is arranged under the overlay mode according to the barrier layer of 2-2 compound, by ferroelectric phase with ferromagnetic to burn altogether in the mode of lamellar composite together with, effectively can suppress reacting to each other thus keeping respective characteristic between two-phase, make it not only have good ferroelectricity but also have good ferromegnetism.Adopt the mode of burning altogether, to avoid in prior art and directly two-phase mixtures is produced the problem of unpredictable phase, and then improve the performance of magnetic electric compound material, and after the method only will obtain two kinds of powder pressing formings, get rid of PVA tackiness agent, then sinter, can product be obtained, so preparation method is simple.
The magnetic electric compound material that the present invention obtains has excellent ferroelectric, dielectric and magnetic electricity performance.When frequency is 20 hertz, matrix material specific inductivity reaches 750 ~ 1400, and dielectric loss is 0.16 ~ 0.31.The saturated polarization P of each component of matrix material
sbe 9.6 ~ 15.3 μ C/cm
2, coercive field E
cbe 20.2 ~ 23.5kV/cm, its saturation magnetization M
sbe 2.4 ~ 6.8emu/g, coercive field H
cbe 73.4 ~ 104.7Oe.
In addition, owing to there is not lead in the raw material that the present invention adopts, so preparation method can not pollute, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode according to the barrier layer of 2-2 compound and is sintered together, and does not need tackiness agent between layers, and thus the transmission of stress-strain can efficiently directly complete.The material compactness that the present invention obtains is good, exist without obvious gross blow hole, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena, interface coupling is better, so the present invention can ensure magnetic electric compound material directly efficient magnetic-electricity-Li efficiency of conversion, thus improves the magnetoelectricity conversion performance of matrix material.
Accompanying drawing explanation
Fig. 1 is lower x BiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3x=0.1 is worked as, 0.2,0.3 in component, when 0.4, the structure iron of composite ceramics when 1100 DEG C of sintering.
Fig. 2 is x BiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.1, the dielectric and magnetic of composite ceramics after 1100 DEG C of sintering.
Fig. 3 is x BiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.2, the dielectric and magnetic of composite ceramics after 1100 DEG C of sintering.
Fig. 4 is x BiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.3, the dielectric and magnetic of composite ceramics after 1100 DEG C of sintering.
Fig. 5 is x BiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.4, the dielectric and magnetic of composite ceramics after 1100 DEG C of sintering.
Fig. 6 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3ferroelectric hysteresis loop in component during x=0.1.
Fig. 7 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3ferroelectric hysteresis loop in component during x=0.2.
Fig. 8 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3ferroelectric hysteresis loop in component during x=0.3.
Fig. 9 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3ferroelectric hysteresis loop in component during x=0.4.
Figure 10 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3magnetic hysteresis loop in component during x=0.1.
Figure 11 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3magnetic hysteresis loop in component during x=0.2.
Figure 12 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3magnetic hysteresis loop in component during x=0.3.
Figure 13 is the ceramic xBiY at 1100 DEG C of sintering
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3magnetic hysteresis loop in component during x=0.4.
Figure 14 is xBiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.1, composite ceramics is at the SEM figure of 1100 DEG C of sintering rear interfaces.
Figure 15 is xBiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.2, composite ceramics is at the SEM figure of 1100 DEG C of sintering rear interfaces.
Figure 16 is xBiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.3, composite ceramics is at the SEM figure of 1100 DEG C of sintering rear interfaces.
Figure 17 is xBiY under room temperature
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.4, composite ceramics is at the SEM figure of 1100 DEG C of sintering rear interfaces.
In figure, 1 is 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder, 2 is BiY
2fe
5o
12powder.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.In the present invention, the barrier layer of 2-2 compound is arranged under the overlay mode and is: together with stacking with the order of ferroelectric phase according to ferroelectric phase, ferromagnetic phase successively from the top down.
Embodiment 1
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.1.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 880 DEG C of pre-burnings 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1020 DEG C of pre-burnings 4 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.1, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 550 DEG C, is incubated 3 hours at 1100 DEG C, sinters 2 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Fig. 1 is x BiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.1, the structure iron of composite ceramics when 1100 DEG C of sintering.
As seen from Figure 2, matrix material has larger specific inductivity, and when 20 hertz, specific inductivity is 1400, and dielectric loss is 0.31.As seen from Figure 6, matrix material has obvious ferroelectricity, and saturated polarization is 15.3 μ C/cm
2, coercive field is 23.5kV/cm.As seen from Figure 10, matrix material has obvious ferromegnetism, and saturation magnetization is 2.4emu/g, and coercive field is 73.4Oe.As can be seen from Figure 14, good in the material compactness of 1100 DEG C of sintering, exist without obvious gross blow hole, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena.
Embodiment 2
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.2.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 920 DEG C of pre-burnings 4 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1000 DEG C of pre-burnings 6 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 15%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 15%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.2, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 580 DEG C, is incubated 4 hours at 1100 DEG C, sinters 3 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Fig. 1 is x BiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.2, the structure iron of composite ceramics when 1100 DEG C of sintering.
As seen from Figure 3, matrix material has larger specific inductivity, and when 20 hertz, specific inductivity is 1250, and dielectric loss is 0.29.As seen from Figure 7, matrix material has obvious ferroelectricity, and saturated polarization is 12.7 μ C/cm
2, coercive field is 21.6kV/cm.As seen from Figure 11, matrix material has obvious ferromegnetism, and saturation magnetization is 3.6emu/g, and coercive field is 88.6Oe.As can be seen from Figure 15, good in the material compactness of 1100 DEG C of sintering, exist without obvious gross blow hole, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena.
Embodiment 3
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.3.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 900 DEG C of pre-burnings 5 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1010 DEG C of pre-burnings 5 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 12%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 12%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.3, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 600 DEG C, is incubated 5 hours at 1100 DEG C, sinters 4 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Fig. 1 is x BiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.3, the structure iron of composite ceramics when 1100 DEG C of sintering.
As seen from Figure 4, matrix material has larger specific inductivity, and when 20 hertz, specific inductivity is 800, and dielectric loss is 0.24.As seen from Figure 8, matrix material has obvious ferroelectricity, and saturated polarization is 10.1 μ C/cm
2, coercive field is 20.4kV/cm.As seen from Figure 12, matrix material has obvious ferromegnetism, and saturation magnetization is 4.1emu/g, and coercive field is 89.3Oe.As can be seen from Figure 16, good in the material compactness of 1100 DEG C of sintering, exist without obvious gross blow hole, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena.
Embodiment 4
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.4.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 4.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 890 DEG C of pre-burnings 5 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 5.5 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1005 DEG C of pre-burnings 5 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 8%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.4, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 560 DEG C, is incubated 4.5 hours at 1100 DEG C, sinters 2.5 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Fig. 1 is x BiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3in component as x=0.4, the structure iron of composite ceramics when 1100 DEG C of sintering.
As seen from Figure 5, matrix material has larger specific inductivity, and when 20 hertz, specific inductivity is 750, and dielectric loss is 0.16.As seen from Figure 9, matrix material has obvious ferroelectricity, and saturated polarization is 9.6 μ C/cm
2, coercive field is 20.2kV/cm.As seen from Figure 13, matrix material has obvious ferromegnetism, and saturation magnetization is 6.8emu/g, and coercive field is 104.7Oe.As can be seen from Figure 17, good in the material compactness of 1100 DEG C of sintering, exist without obvious gross blow hole, two-phase even grain size, all at systems, without obvious interface atoms diffusion phenomena.
Embodiment 5
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.15.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 900 DEG C of pre-burnings 4.5 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1000 DEG C of pre-burnings 5.5 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 13%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 13%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.15, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 590 DEG C, is incubated 3 hours at 1150 DEG C, sinters 3.5 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Embodiment 6
The chemical formula of layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.35.
The preparation method of above-mentioned layered electromagnetic matrix material, comprises the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3within 4 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 910 DEG C of pre-burnings 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3within 6 hours, mixed by wet ball grinding after preparation, then dry, sieve, briquetting, then through 1020 DEG C of pre-burnings 4 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
30.65BaTiO is added in powder
3-0.35 (Na
0.5bi
0.5) TiO
3granulation after the PVA tackiness agent of powder quality 13%, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12biY is added in powder
2fe
5o
12granulation after the PVA tackiness agent of powder quality 13%, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder; Wherein, PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.35, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound; Wherein, the barrier layer of 2-2 compound is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder 1, BiY
2fe
5o
12powder 2,0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder 1 stacks together.
(5) at temperature is 600 DEG C, is incubated 4 hours at 1020 DEG C, sinters 3 hours one-tenth porcelain again after eliminating PVA tackiness agent, obtain layered electromagnetic matrix material.
Claims (9)
1. a layered electromagnetic matrix material, is characterized in that, the chemical formula of this layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.4.
2. layered electromagnetic matrix material according to claim 1, is characterized in that, the chemical formula of this layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.2.
3. layered electromagnetic matrix material according to claim 1, is characterized in that, the chemical formula of this layered electromagnetic matrix material is: xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and x=0.1.
4. the preparation method of layered electromagnetic matrix material according to claim 1, is characterized in that, comprise the following steps:
(1) by chemical formula 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3by analytically pure BaCO
3, TiO
2, Bi
2o
3, Na
2cO
3mixed by ball milling after preparation, then sieve, briquetting, then through 880 ~ 920 DEG C of pre-burnings 4 ~ 6 hours, obtain bulk product, cross 120 mesh sieves after then bulk product being pulverized and obtain 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder;
(2) by chemical formula formula BiY
2fe
5o
12by analytically pure Bi
2o
3, Y
2o
3, Fe
2o
3mixed by ball milling after preparation, then sieve, briquetting, then through 1000 ~ 1020 DEG C of pre-burnings 4 ~ 6 hours, obtain blocks of solid, cross 120 mesh sieves after then being pulverized by blocks of solid and obtain BiY
2fe
5o
12powder;
(3) to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain the 0.65BaTiO of uniform particle sizes
3-0.35 (Na
0.5bi
0.5) TiO
3powder; To BiY
2fe
5o
12add granulation after PVA tackiness agent in powder, then sieve through 60 eye mesh screens, obtain the BiY of uniform particle sizes
2fe
5o
12powder;
(4) according to chemical formula xBiY
2fe
5o
12/ (1-x) 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3, wherein x is BiY
2fe
5o
12mass percent, and 0.1≤x≤0.4, by 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder and BiY
2fe
5o
12powder is arranged under the overlay mode compression moulding in a mold according to the barrier layer of 2-2 compound;
(5) at 1100 ~ 1150 DEG C, sinter 2 ~ 4 hours again after getting rid of PVA tackiness agent and become porcelain, obtain layered electromagnetic matrix material.
5. the preparation method of layered electromagnetic matrix material according to claim 4, is characterized in that, in described step (1), step (4), Ball-milling Time is 4 ~ 6 hours.
6. the preparation method of layered electromagnetic matrix material according to claim 4, is characterized in that, to 0.65BaTiO in described step (3)
3-0.35 (Na
0.5bi
0.5) TiO
3the quality adding PVA tackiness agent in powder is 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
38% ~ 15% of powder quality; To BiY
2fe
5o
12the quality adding PVA tackiness agent in powder is BiY
2fe
5o
128% ~ 15% of powder quality.
7. the preparation method of the layered electromagnetic matrix material according to claim 4 or 6, is characterized in that, described PVA tackiness agent is the polyvinyl alcohol water solution of massfraction 10%.
8. the preparation method of the layered electromagnetic matrix material according to claim 4 or 6, is characterized in that, the barrier layer of the middle 2-2 compound of described step (4) is arranged under the overlay mode and is specially: from the top down according to 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3powder, BiY
2fe
5o
12powder, 0.65BaTiO
3-0.35 (Na
0.5bi
0.5) TiO
3the order of powder stacks together.
9. the preparation method of the layered electromagnetic matrix material according to claim 4 or 6, is characterized in that, described eliminating PVA tackiness agent specifically: at temperature is 550-600 DEG C, be incubated 3-5 hour.
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CN108569897A (en) * | 2017-03-09 | 2018-09-25 | Tdk株式会社 | Piezoelectric composition and piezoelectric element |
CN110981466A (en) * | 2019-11-29 | 2020-04-10 | 湖南工程学院 | Interface coupling enhanced layered magnetoelectric composite ceramic and preparation method thereof |
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