CN106278252A - A kind of bismuth titanates Bi4 Xprxti3 Xcoxo12ceramic material and preparation method thereof - Google Patents

A kind of bismuth titanates Bi4 Xprxti3 Xcoxo12ceramic material and preparation method thereof Download PDF

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CN106278252A
CN106278252A CN201610648814.5A CN201610648814A CN106278252A CN 106278252 A CN106278252 A CN 106278252A CN 201610648814 A CN201610648814 A CN 201610648814A CN 106278252 A CN106278252 A CN 106278252A
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ceramic material
preparation
bismuth titanates
powder
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杨海波
孙雨佳
林营
张晓婕
朱建锋
王芬
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Shaanxi University of Science and Technology
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Abstract

A kind of bismuth titanates Bi4‑xPrxTi3‑xCoxO12Ceramic material and preparation method thereof, by solid phase method by Bi2O3、TiO2、Pr2O3、Co3O4Carrying out dispensing in molar ratio, x is dopant ion Pr3+And Co3+The mole percent of ion.After mix homogeneously at 700～800 DEG C pre-burning 4～8h, then secondary ball milling, pelletize, the most compressing, discharge PVA binding agent, microwave sintering at 920～1000 DEG C, be incubated 20～40min.Owing to bismuth titanates is carried out Pr in the present invention3+And Co3+The doping of AB position, improving while its ferroelectric properties, introducing and improve the ferromagnetic property of material.And use the mode of microwave sintering, it is achieved low temperature Fast Sintering, prepare and have high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4‑xPrxTi3‑ xCoxO12Ceramic material.

Description

A kind of bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material and preparation method thereof
Technical field
The invention belongs to material science, relate to a kind of bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material and preparation thereof Method.
Background technology
Simultaneously developing rapidly along with computer technology and electronic information technology, the requirement of electronic devices and components is more come by people The highest so that various electronic equipments become being more highly integrated, multifunction, miniaturization and quickly response, electronic equipment Electronic information exchange and storage system all less towards volume, the faster direction of storage speed is developed.So, cause single group The material divided often is difficult to competent requirement, and a kind of new material of eager needs has higher performance or has two kinds or two simultaneously Plant above performance, to reduce the electronic devices and components consumption in the circuit board confined space, realize the miniaturization of device, base further In this, there is ferroelectricity simultaneously and ferromagnetic ceramic material arises at the historic moment.
But, the kind of magnetoelectricity monophase materials is considerably less.Even and if its magnetoelectric induction is the faintest.Pottery Material not only has ferroelectricity and ferromagnetism, and can produce magneto-electric coupled function, greatly by the coupling synergism of ferrum Widened greatly the range of application of ferroic material, the components and parts utilizing multi-ferroic material to make have conversion, transmit, process information, Storage energy, save the function such as the energy, be widely used in the energy, telecommunications, automatically control, communication, household electrical appliance, biology, doctor Treat the fields such as health, light industry, ore dressing, physics mine locating, military project.
Bismuth titanates (Bi4Ti3O12) it is the perovskite-like structure ferroelectric material of a kind of function admirable, there is high-curie temperature Point, preferable frequency stability, the advantage such as excellent anisotropy and special electrical property has obtained paying close attention to widely.? Proof can introduce ferromagnetic property by bismuth titanates carries out the magnetic ion doping of B position, but can greatly reduce material electricity simultaneously Resistance rate, deteriorates the ferroelectric properties of material, thus affects range of application (Palkar V R, the Malik S of material K.Observation of magnetoelectric behavior at room temperature in Pb(Fe1-xTix)O3 [J].Solid State Communications,2005,134(11):783-786.)；(Liu Y,Pu Y,Sun Z.Correlation between lattice distortion and magnetic and electrical properties of Fe-doped Bi4Ti3O12ceramics[J].Journal of Materials Science Materials in Electronics,2015,26(10):7484-7489.)。
Summary of the invention
It is an object of the invention to provide a kind of bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material and preparation method thereof, should In method, sintering temperature is low, and sintering rate is fast, along with Pr3+And Co3+The increase of doping, ferroelectricity, ferromagnetism are significantly carried High.Disruptive field intensity is 175kV/cm, and saturated polarization is 21.3～25.1 μ C/cm2, saturation magnetization be 8.3～ 23.2memu/g。
For achieving the above object, the present invention adopts the following technical scheme that:
A kind of bismuth titanates Bi4-xPrxTi3-xCoxO12The preparation method of ceramic material, comprises the following steps:
1) chemical formula Bi is pressed4-xPrxTi3-xCoxO12By Bi2O3、TiO2、Pr2O3And Co3O4By mix homogeneously after preparation, so Post-drying, sieves, pre-burning 4～8h at 700～800 DEG C, crosses 120 mesh sieves and obtain Bi after ball milling4-xPrxTi3-xCoxO12Powder body； Wherein, x is dopant ion Pr3+And Co3+The mole percent of ion, and 0.1≤x≤0.3；
2) by Bi4-xPrxTi3-xCoxO12After powder body pelletize, then sieve through 60 eye mesh screens, obtain the Bi of uniform particle sizes4- xPrxTi3-xCoxO12Powder；
3) by Bi4-xPrxTi3-xCoxO12After powder pressing forming, microwave sintering at 920～1000 DEG C, insulation 20～ 40min, obtains bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material.
The present invention is further improved by, Bi2O3、TiO2、Pr2O3And Co3O4It is analytical pure.
The present invention is further improved by, and mix homogeneously is realized by ball milling, and the time of ball milling be 10～ 12 hours.
The present invention is further improved by, ball milling post-drying, and the temperature of drying is 80～100 DEG C, and the time of drying is 8 ～12 hours.
The present invention is further improved by, by Bi4-xPrxTi3-xCoxO12Powder body pelletize detailed process is as follows: to Bi4- xPrxTi3-xCoxO12Adding pelletize after PVA binding agent in powder body, wherein, the quality adding PVA binding agent is Bi4-xPrxTi3- xCoxO12The 8%～12% of powder quality.
The present invention is further improved by, and PVA binding agent is mass fraction 8～the polyvinyl alcohol water solution of 10%.
The present invention is further improved by, compressing specifically by Bi4-xPrxTi3-xCoxO12Powder is placed in mould In, then in powder compressing machine, compacting pressurize 1～3 minutes under 3～6MPa.
The present invention is further improved by, microwave sintering at 920～1000 DEG C.
The present invention is further improved by, and the temperature getting rid of PVA binding agent is 500～600 DEG C, and the time is 4～6 little Time.
A kind of bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material, the chemical formula of this ceramic material is: Bi4-xPrxTi3- xCoxO12, wherein x dopant ion is Pr3+And Co3+The mole percent of ion, and 0.1≤x≤0.3.
The present invention is further improved by, 0.1≤x≤0.2.
The present invention is further improved by, x=0.1.
Compared with prior art, the invention have the benefit that and prepare Bi by conventional solid-state method4-xPrxTi3- xCoxO12Powder body.Wherein, x is dopant ion Pr3+And Co3+The mole percent of ion, and 0.1≤x≤0.3.By chemical formula Bi4-xPrxTi3-xCoxO12By analytically pure Bi2O3、TiO2、Pr2O3And Co3O4Mixed by ball milling after preparing according to certain mol proportion Close uniformly, then dry, sieve, pre-burning, cross 120 mesh sieves after ball milling and obtain Bi4-xPrxTi3-xCoxO12Powder body；Pelletize, then through 60 Eye mesh screen sieves, and obtains the Bi of uniform particle sizes4-xPrxTi3-xCoxO12Powder, and by after compressing for mixed-powder, 900～ 1000 DEG C of microwave sinterings, are incubated 20～40min, obtain high ferroelectricity high-ferromagnetic Bi4-xPrxTi3-xCoxO12Ceramic material.
In the present invention, bismuth titanate ceramics material uses microwave sintering method, relies on material itself absorb microwave energy and be converted into material The kinetic energy of material interior molecules and potential energy, make the inside and outside the most uniformly heating of material, and the thermal stress that therefore material internal is formed is minimum.This Outward, under the effect of microwave electromagnetic energy, the kinetic energy of material internal molecule (or ion) increases, and makes sintering activating energy reduce, diffusion Coefficient improves, and therefore can realize low temperature Fast Sintering, makes micropowder crystal grain have little time to grow up the most and completes sintering, thus prepares guarantor Hold the sintered body of fine-grain.The present invention is compared with solid-phase sintering, and sintering time is short, saves the energy, reduces cost, and After sintering, crystal grain is tiny, and material compactness is good, and refers to that preparation method is simple.
By Pr position rare earth-doped to A in the present invention3+Ion, significantly improves the ferroelectric properties of material.Simultaneously to B position magnetic Property doping Co3+Ion, makes material be provided simultaneously with room temperature high-ferromagnetic.Prepare bismuth titanate ceramics material have excellence ferroelectricity and Ferromagnetic property.Disruptive field intensity is 175kV/cm, and saturated polarization is 21.3～25.1 μ C/cm2, saturation magnetization is 8.3 ～23.2memu/g.
It addition, due to the most leaded in the raw material of present invention employing, so preparation method does not results in pollution, can in this material Adjust doping content within the specific limits, need to prepare the ceramic material of respective performances according to difference.Due to resistivity of material The highest so that the leakage conductance electric current of material entirety is less, beneficially material ferroelectricity and the raising of ferromagnetic property.The present invention prepares Material compactness is good, exists without obvious gross blow hole, even grain size, all in micron number magnitude.Sintering temperature is low, technique letter Single, save the energy, reduce cost.
Accompanying drawing explanation
Fig. 1 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The XRD figure of ceramic material.
Fig. 2 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The XRD figure of ceramic material.
Fig. 3 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The XRD figure of ceramic material.
Fig. 4 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The room temperature ferroelectric hysteresis loop figure of ceramic material.
Fig. 5 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The room temperature ferroelectric hysteresis loop figure of ceramic material.
Fig. 6 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The room temperature ferroelectric hysteresis loop figure of ceramic material.
Fig. 7 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The room temperature hysteresis curve figure of ceramic material.
Fig. 8 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The room temperature ferroelectric hysteresis loop figure of ceramic material.
Fig. 9 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The room temperature ferroelectric hysteresis loop figure of ceramic material.
Figure 10 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The SEM figure of ceramic material.
Figure 11 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The SEM figure of ceramic material.
Figure 12 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The SEM figure of ceramic material.
Detailed description of the invention
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
Compressing in the present invention specifically powder is placed in mould, then in powder compressing machine, presses under 3～6MPa System pressurize 1～3 minutes.
Embodiment 1
One has high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4-xPrxTi3-xCoxO12Ceramic material, chemical expression is Bi4-xPrxTi3-xCoxO12, wherein x is dopant ion Pr3+And Co3+The mole percent of ion, and x=0.1.
Above-mentioned Bi3.9Pr0.1Ti2.9Co0.1O12The preparation method of ceramic material, comprises the following steps:
1) chemical formula Bi is pressed3.9Pr0.1Ti2.9Co0.1O12By analytically pure Bi2O3、TiO2、Pr2O3And Co3O4According to mol ratio By ball milling mix homogeneously after preparation, Ball-milling Time is 10 hours, then dries, and the temperature being dried is 100 DEG C, the time being dried It it is 8 hours.Sieve, through 800 DEG C of pre-burnings 4 hours, cross 120 mesh sieves after secondary ball milling, obtain Bi3.9Pr0.1Ti2.9Co0.1O12Powder body；
2) to Bi3.9Pr0.1Ti2.9Co0.1O12Adding pelletize after PVA binding agent in powder body, PVA binding agent is mass fraction The polyvinyl alcohol water solution of 8%, the quality adding PVA binding agent is Bi3.9Pr0.1Ti2.9Co0.1O12The 12% of powder quality.Again Sieve through 60 eye mesh screens, obtain the Bi of uniform particle sizes3.9Pr0.1Ti2.9Co0.1O12Powder；
3) by Bi3.9Pr0.1Ti2.9Co0.1O12Powder is positioned in mould, then in powder compressing machine, suppresses under 6MPa And pressurize 1 minute, compressing after, get rid of PVA binding agent, dump temperature is 600 DEG C, and the binder removal time is 4 hours.Then exist 920 DEG C of microwave sinterings, are incubated 35min, obtain high ferroelectricity high-ferromagnetic Bi3.9Pr0.1Ti2.9Co0.1O12Ceramic material.
Fig. 1 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The XRD figure of ceramic material.Sintering process is burnt During knot, crystal structure is in order, generates without dephasign.
Fig. 4 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The room temperature ferroelectric hysteresis loop figure of ceramic material.Material Material has the ferroelectric properties of excellence, and disruptive field intensity is 175kV/cm, and saturated polarization is 21.3 μ C/cm2。
Fig. 7 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The room temperature hysteresis curve figure of ceramic material.Material Material has obvious ferromagnetic property, and saturation magnetization is 8.3memu/g.
Figure 10 is 920 DEG C of sintering 35min gained Bi3.9Pr0.1Ti2.9Co0.1O12The SEM figure of ceramic material.Crystal grain presents circle Disk-like structure, compactness is good, exists without obvious gross blow hole, and size is in micron number magnitude.
Embodiment 2
One has high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4-xPrxTi3-xCoxO12Ceramic material, chemical expression is Bi4-xPrxTi3-xCoxO12, wherein x is dopant ion Pr3+And Co3+The mole percent of ion, and x=0.2.
Above-mentioned Bi3.8Pr0.2Ti2.8Co0.2O12The preparation method of ceramic material, comprises the following steps:
1) chemical formula Bi is pressed3.8Pr0.2Ti2.8Co0.2O12By analytically pure Bi2O3、TiO2、Pr2O3And Co3O4According to necessarily rubbing You pass through ball milling mix homogeneously than after preparation, and Ball-milling Time is 12 hours.Then drying, the temperature being dried is 90 DEG C, is dried Time is 10 hours.Sieve, through 750 DEG C of pre-burnings 6 hours, cross 120 mesh sieves after secondary ball milling and obtain Bi3.8Pr0.2Ti2.8Co0.2O12 Powder body；
2) to Bi3.8Pr0.2Ti2.8Co0.2O12Adding pelletize after PVA binding agent in powder body, PVA binding agent is mass fraction The polyvinyl alcohol water solution of 9%, the quality adding PVA binding agent is Bi3.8Pr0.2Ti2.8Co0.2O12The 10% of powder quality.Again Sieve through 60 eye mesh screens, obtain the Bi of uniform particle sizes3.8Pr0.2Ti2.8Co0.2O12Powder；
3) by Bi3.8Pr0.2Ti2.8Co0.2O12Powder is positioned in mould, then in powder compressing machine, suppresses under 3MPa And pressurize 3 minutes, compressing after, get rid of PVA binding agent, dump temperature is 550 DEG C, and the binder removal time is 5 hours.Then exist 950 DEG C of microwave sinterings, are incubated 30min, obtain high ferroelectricity high-ferromagnetic Bi3.8Pr0.2Ti2.8Co0.2O12Ceramic material.
Fig. 2 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The XRD figure of ceramic material.Crystalline substance in sintering process Body crystalline condition is good, generates without dephasign.
Fig. 5 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The room temperature ferroelectric hysteresis loop figure of ceramic material.Material Material has the ferroelectric properties of excellence, and disruptive field intensity is 175kV/cm, and saturated polarization is 22.2 μ C/cm2。
Fig. 8 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The room temperature hysteresis curve figure of ceramic material.Material Material has obvious ferromagnetic property, and saturation magnetization is 12.7memu/g.
Figure 11 is 950 DEG C of sintering 30min gained Bi3.8Pr0.2Ti2.8Co0.2O12The SEM figure of ceramic material.Crystal grain presents circle Disk-like structure, compactness is good, exists without obvious gross blow hole, and size is in micron number magnitude.
Embodiment 3
One has high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4-xPrxTi3-xCoxO12Ceramic material, chemical expression is Bi4-xPrxTi3-xCoxO12, wherein x is dopant ion Pr3+And Co3+The mole percent of ion.And x=0.3.
Above-mentioned Bi3.7Pr0.3Ti2.7Co0.3O12The preparation method of ceramic material, comprises the following steps:
1) chemical formula Bi is pressed3.7Pr0.3Ti2.7Co0.3O12By analytically pure Bi2O3、TiO2、Pr2O3And Co3O4According to mol ratio By ball milling mix homogeneously after preparation, Ball-milling Time is 12 hours.Then drying, the temperature being dried is 80 DEG C, the time being dried It it is 12 hours.Sieve, through 700 DEG C of pre-burnings 8 hours, cross 120 mesh sieves after secondary ball milling and obtain Bi3.7Pr0.3Ti2.7Co0.3O12Powder body；
2) to Bi3.7Pr0.3Ti2.7Co0.3O12Adding pelletize after PVA binding agent in powder body, PVA binding agent is mass fraction The polyvinyl alcohol water solution of 10%, the quality adding PVA binding agent is Bi3.7Pr0.3Ti2.7Co0.3O12The 8% of powder quality.Again Sieve through 60 eye mesh screens, obtain the Bi of uniform particle sizes3.7Pr0.3Ti2.7Co0.3O12Powder；
3) by Bi3.7Pr0.3Ti2.7Co0.3O12Powder is positioned in mould, then in powder compressing machine, suppresses under 5MPa And pressurize 2 minutes, compressing after, get rid of PVA binding agent, dump temperature is 500 DEG C, and the binder removal time is 6 hours.Then exist 1000 DEG C of microwave sinterings, are incubated 20min, obtain high ferroelectricity high-ferromagnetic Bi3.7Pr0.3Ti2.7Co0.3O12Ceramic material.
Fig. 3 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The XRD figure of ceramic material.In sintering process Crystal structure in order, generates without dephasign.
Fig. 6 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The room temperature ferroelectric hysteresis loop figure of ceramic material.Material Material has the ferroelectric properties of excellence, and disruptive field intensity is 175kV/cm, and saturated polarization is 25.1 μ C/cm2。
Fig. 9 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The room temperature hysteresis curve figure of ceramic material.Material Material has obvious ferromagnetic property, and saturation magnetization is 23.2memu/g.
Figure 12 is 1000 DEG C of sintering 20min gained Bi3.7Pr0.3Ti2.7Co0.3O12The SEM figure of ceramic material.Crystal grain presents circle Disk-like structure, compactness is good, exists without obvious gross blow hole, and size is in micron number magnitude.
Embodiment 4
One has high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4-xPrxTi3-xCoxO12Ceramic material, chemical expression is Bi4-xPrxTi3-xCoxO12, wherein x is dopant ion Pr3+And Co3+The mole percent of ion, and x=0.2.
Above-mentioned Bi3.8Pr0.2Ti2.8Co0.2O12The preparation method of ceramic material, comprises the following steps:
1) chemical formula Bi is pressed3.8Pr0.2Ti2.8Co0.2O12By analytically pure Bi2O3、TiO2、Pr2O3And Co3O4According to necessarily rubbing You pass through ball milling mix homogeneously than after preparation, and Ball-milling Time is 11 hours.Then drying, the temperature being dried is 85 DEG C, is dried Time is 9 hours.Sieve, through 780 DEG C of pre-burnings 7 hours, cross 120 mesh sieves after secondary ball milling and obtain Bi3.8Pr0.2Ti2.8Co0.2O12Powder Body；
2) to Bi3.8Pr0.2Ti2.8Co0.2O12Adding pelletize after PVA binding agent in powder body, PVA binding agent is mass fraction The polyvinyl alcohol water solution of 8%, the quality adding PVA binding agent is Bi3.8Pr0.2Ti2.8Co0.2O12The 9% of powder quality.Warp again 60 eye mesh screens sieve, and obtain the Bi of uniform particle sizes3.8Pr0.2Ti2.8Co0.2O12Powder；
3) by Bi3.8Pr0.2Ti2.8Co0.2O12Powder is positioned in mould, then in powder compressing machine, suppresses under 4MPa And pressurize 3 minutes, compressing after, get rid of PVA binding agent, dump temperature is 520 DEG C, and the binder removal time is 6 hours.Then exist 930 DEG C of microwave sinterings, are incubated 40min, obtain high ferroelectricity high-ferromagnetic Bi3.8Pr0.2Ti2.8Co0.2O12Ceramic material.
The present invention provides one to have high ferroelectricity high-ferromagnetic bismuth titanates Bi concurrently4-xPrxTi3-xCoxO12Ceramic material and Preparation method.Using microwave sintering method to prepare in the method, technique is simple, and sintering temperature is low, and material compactness is good, stability High.Along with Pr3+And Co3+The increase of doping, the ferroelectricity of material, ferromagnetism are significantly improved.
While the present invention by carrying out the magnetic ion doping of B position to bismuth titanates, its A position is carried out rare earth ion doped next Improve the ferroelectric properties of bismuth titanates so that bismuth titanate ceramics material is also equipped with higher ferrum simultaneously while having high ferroelectric properties Magnetic property.Pass through Pr3+Replace Bi3+、Co3+Replace Ti4+Bismuth titanates is doped modification, significantly improves its room temperature ferroelectricity And ferromagnetism.Bi4-xPrxTi3-xCoxO12Ceramic material utilizes microwave sintering method, and technique is simple, and has low temperature Fast Sintering Advantage, to high ferroelectricity high-ferromagnetic bismuth titanates Bi4-xPrxTi3-xCoxO12Preparation and the performance study of ceramic material provide Important premise.

Claims (10)

1. a bismuth titanates Bi4-xPrxTi3-xCoxO12The preparation method of ceramic material, it is characterised in that comprise the following steps:
1) chemical formula Bi is pressed4-xPrxTi3-xCoxO12By Bi2O3、TiO2、Pr2O3And Co3O4By mix homogeneously, then mistake after preparation Sieve, pre-burning 4～8h at 700～800 DEG C, cross 120 mesh sieves after ball milling and obtain Bi4-xPrxTi3-xCoxO12Powder body；Wherein, x is for mixing Heteroion Pr3+And Co3+The mole percent of ion, and 0.1≤x≤0.3；
2) by Bi4-xPrxTi3-xCoxO12After powder body pelletize, then sieve through 60 eye mesh screens, obtain the Bi of uniform particle sizes4-xPrxTi3- xCoxO12Powder；
3) by Bi4-xPrxTi3-xCoxO12After powder pressing forming, microwave sintering at 920～1000 DEG C, it is incubated 20～40min, Obtain bismuth titanates Bi4-xPrxTi3-xCoxO12Ceramic material.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, Bi2O3、TiO2、Pr2O3And Co3O4It is analytical pure.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, mix homogeneously is realized by ball milling, and the time of ball milling is 10～12 hours.
A kind of bismuth titanates Bi the most according to claim 24-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, ball milling post-drying, the temperature of drying is 80～100 DEG C, and the time of drying is 8～12 hours.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, by Bi4-xPrxTi3-xCoxO12Powder body pelletize detailed process is as follows: to Bi4-xPrxTi3-xCoxO12Powder body adds PVA bonding Pelletize after agent, wherein, the quality adding PVA binding agent is Bi4-xPrxTi3-xCoxO12The 8%～12% of powder quality.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, PVA binding agent is mass fraction 8～the polyvinyl alcohol water solution of 10%.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, compressing specifically by Bi4-xPrxTi3-xCoxO12Powder is placed in mould, then in powder compressing machine, and 3～6MPa Lower compacting pressurize 1～3 minutes.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, microwave sintering at 920～1000 DEG C.
A kind of bismuth titanates Bi the most according to claim 14-xPrxTi3-xCoxO12The preparation method of ceramic material, its feature exists In, the temperature getting rid of PVA binding agent is 500～600 DEG C, and the time is 4～6 hours.
10. the bismuth titanates Bi that according to claim 1 prepared by method4-xPrxTi3-xCoxO12Ceramic material, its feature exists In, the chemical formula of this ceramic material is: Bi4-xPrxTi3-xCoxO12, wherein x dopant ion is Pr3+And Co3+Moles the hundred of ion Mark, and 0.1≤x≤0.3.
CN201610648814.5A 2016-08-09 2016-08-09 A kind of bismuth titanates Bi4 Xprxti3 Xcoxo12ceramic material and preparation method thereof Pending CN106278252A (en)

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CN110092658A (en) * 2019-05-31 2019-08-06 新乡学院 A kind of preparation method of bismuth system ceramics
CN116332641A (en) * 2023-04-07 2023-06-27 广西华锡集团股份有限公司 Yb-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108117387A (en) * 2018-01-04 2018-06-05 陕西科技大学 A kind of New Co and Fe are co-doped with Bi4Ti3O12Multiferroic and magnetic dielectric ceramic material and preparation method thereof
CN110092658A (en) * 2019-05-31 2019-08-06 新乡学院 A kind of preparation method of bismuth system ceramics
CN116332641A (en) * 2023-04-07 2023-06-27 广西华锡集团股份有限公司 Yb-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof
CN116332641B (en) * 2023-04-07 2024-04-12 广西华锡集团股份有限公司 Yb-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof

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