CN115231915A - Preparation method of compact impurity-free bismuth ferrite-strontium titanate ceramic material - Google Patents
Preparation method of compact impurity-free bismuth ferrite-strontium titanate ceramic material Download PDFInfo
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- CN115231915A CN115231915A CN202210844933.3A CN202210844933A CN115231915A CN 115231915 A CN115231915 A CN 115231915A CN 202210844933 A CN202210844933 A CN 202210844933A CN 115231915 A CN115231915 A CN 115231915A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 58
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 229910002367 SrTiO Inorganic materials 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 36
- 230000005684 electric field Effects 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 12
- 238000000748 compression moulding Methods 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000005553 drilling Methods 0.000 claims description 8
- 238000000462 isostatic pressing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052845 zircon Inorganic materials 0.000 claims description 8
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000011267 electrode slurry Substances 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 210000000988 bone and bone Anatomy 0.000 claims description 2
- 238000009694 cold isostatic pressing Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 229910052697 platinum Inorganic materials 0.000 description 12
- 239000012071 phase Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000003825 pressing Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a compact non-hetero-phase bismuth ferrite-strontium titanate ceramic material according to BiFeO 3 With SrTiO 3 Weighing raw materials according to the mass ratio of 3 2 And after the preset current lasts for 60s, the sintering is finished; the invention realizes the ceramic by using the joule heat under the action of the electric fieldThe required sintering time is very short, the preparation of the nano-sized ceramic material is realized, the micro-morphology and the physical and chemical properties of the material are optimized, and the uniform and compact ceramic material without impurity phases is finally prepared.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a preparation method of a compact impurity-free bismuth ferrite-strontium titanate ceramic material.
Background
In the development process of materials for thousands of years, ceramic is used as a unique material with high strength, high hardness, high stability and corrosion resistance, and is widely applied to various aspects such as aerospace, military, electronics, industry and the like. However, in the application of ceramic materials, the main problem is that the ceramic materials are difficult to sinter, and the requirement of densification can be met from a ceramic blank to an advanced ceramic material with specific properties through a long-time high-temperature sintering process, so that the industrial production of the ceramic is in the situation of low efficiency, high energy consumption and high cost for a long time. The long-term high-temperature treatment inevitably causes a problem of significant grain growth, resulting in deterioration of material properties. The traditional ceramic sintering method is energy-consuming and time-consuming in production process. Without careful process control, the high temperatures required for high densities can cause the initial particle size to start growing significantly, making it difficult to maintain a nano-sized grain structure even with nanocrystalline starting materials.
The current research shows that BiFeO 3 SrTiO doped ceramics 3 And the energy storage efficiency and the energy storage density can be improved. Meanwhile, srTiO 3 Can improve BiFeO 3 The stability of the high-voltage-stability ferroelectric capacitor is that MPB (morphotropic phase boundary) is constructed on a BFO-STO matrix, and tetragonal and rhombohedral phases exist at the same time, so that the optimization of ferroelectric and piezoelectric properties can be realized. However, the traditional sintering technology does not solve the problem that the second phase and other sintering problems are easy to occur due to volatilization of Bi and change of Fe valence state in the sintering process of BFO-STO matrix ceramic.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a compact impurity-free bismuth ferrite-strontium titanate ceramic material, which realizes the preparation of a nano-sized ceramic material, optimizes the micro-morphology and the physical and chemical properties of the material, and finally prepares the ceramic material which is uniformly compact and has no impurity phase.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a compact impurity-free bismuth ferrite-strontium titanate ceramic material comprises the following steps:
step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 2 Mixing, and adding 0.1wt% MnO to the mixture 2 Mixing, ball milling, drying and sieving to obtain mixed powder with uniform size;
step two, pouring the obtained mixed powder into a dog-bone-shaped mould for compression moulding, and demoulding the moulded green body to obtain a green body with a perfect shape;
step three, the blank prepared in the step two is cold and is pressed and formed through isostatic pressing;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on a parallel platinum wire through the two holes, connecting the other end of the platinum wire with a power supply, and integrally placing the sample and the platinum wire in a tubular furnace;
step five, rapidly heating the tube furnace to 510-620 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 100-300V/cm, wherein the preset current density is 50mA/mm 2 After keeping for 30-60 s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing and cleaning the sintered ceramic prepared in the step five, coating silver electrode slurry on the surface of the sintered ceramic, then placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic for 10 to 20min at the temperature of 580 to 600 ℃ in the air atmosphere to obtain the compact impurity-free BFO-STO ceramic material.
The invention also has the following technical characteristics:
preferably, in the first step, the raw materials, zircon and deionized water are mixed according to a mass ratio of 1.
Furthermore, the number of the screening meshes in the step one is 120 meshes.
Furthermore, the drying in the first step is drying at the temperature of 80 ℃ for 24 hours.
Preferably, the mold in the second step is a dog bone shape with a size of 20mm × 3.1mm × 1.4mm, and 0.8g of the mixed powder is weighed and poured into a grinding tool for compression molding.
Preferably, the pressure of the cold isostatic pressing in the third step is 200-250 MPa, and the pressure is maintained for 3-5 min.
Preferably, the grinding in the sixth step is to grind the thickness of the sample to 0.3mm by using 240-mesh sand paper, and then grind the front and back surfaces of the sample to 0.2mm by using 2000-mesh sand paper.
Preferably, the cleaning in the sixth step is ultrasonic cleaning in distilled water for 3-5 min.
Compared with the prior art, the invention has the following technical effects:
according to the invention, low-temperature sintering of the ceramic is realized by using joule heat under the action of an electric field, the required sintering time is extremely short, the loss of volatile elements is inhibited, the stoichiometric ratio balance is ensured, the generation of impurity phases is reduced, meanwhile, the grain growth of the ceramic is inhibited under the condition of keeping high densification, and the dense and uniform BFO-STO ceramic is obtained; the energy consumption in the preparation process is low, the service time is short, and the sintering temperature is low, so that a novel preparation method of the energy-saving lead-free energy storage material is provided;
the calcination mode of the invention is a non-equilibrium sintering process, which is determined by extremely high heating rate and short process time in the sintering process, the extremely fast sintering rate ensures that volatile ions cannot reach volatilization and ions which are easy to change valence cannot reach enough heat valence change, thereby realizing the simultaneous occurrence of solid phase reaction and sintering, reducing energy consumption, simultaneously solving the problems of volatilization of Bi ions and valence change of Fe ions in the BFO-STO-based ceramic sintering process and further realizing the optimization of electrical properties;
the invention has simple process equipment, does not need large or complex professional equipment, can realize sintering only in the traditional tube furnace or muffle furnace, saves energy and time in the whole preparation process, is an environment-friendly preparation process, and has high practical value in future industrial production.
Drawings
FIG. 1 is a graph showing the variation of electric field intensity with furnace temperature during sintering at different electric field intensities;
FIG. 2 is a graph showing the variation of current density with furnace temperature during sintering at different electric field strengths;
FIG. 3 is a relationship between the furnace temperature and the electric field;
FIG. 4 is an XRD pattern of the products prepared in examples 2-5;
FIG. 5 is a graph of dielectric constant and dielectric loss as a function of temperature for the products prepared in examples 2-5 at different electric field strengths at a frequency of 1 MHz;
FIG. 6 is a complex impedance plot at 260 ℃ for the products prepared in examples 2-5.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1
Step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 Mixing and then adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1;
step two, pouring the obtained mixed powder into a dog-bone-shaped mold with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression molding, and demolding the molded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing on the blank prepared in the step two by cooling, applying pressure of 2000MPa, and maintaining the pressure for 5min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on the parallel platinum wires through the two holes, connecting the other ends of the platinum wires with a power supply, and integrally placing the sample and the platinum wires in a tubular furnace;
step five, connecting the tube typeThe temperature of the furnace is rapidly raised to 620 ℃ at the heating rate of 10 ℃/min, the sample is kept at the temperature for 30min and then a constant electric field of 100V/cm is applied, and the preset current density is 50mA/mm 2 After keeping for 30s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing the thickness of the sintered ceramic prepared in the step five to 0.3mm by using 240-mesh abrasive paper, then polishing the front side and the back side of the sintered ceramic to 0.2mm by using 2000-mesh abrasive paper, placing the sintered ceramic in distilled water for ultrasonic cleaning for 5min, coating silver electrode slurry on the surface of the sintered ceramic, placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic at 580 ℃ for 20min in an air atmosphere to obtain the compact impurity-phase-free BFO-STO ceramic material.
Example 2
Step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 Mixing and then adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1;
step two, pouring the obtained mixed powder into a dog-bone-shaped mold with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression molding, and demolding the molded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing forming on the blank prepared in the step two in a cold state, applying pressure of 250MPa, and maintaining the pressure for 3min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on a parallel platinum wire through the two holes, connecting the other end of the platinum wire with a power supply, and integrally placing the sample and the platinum wire in a tubular furnace;
step five, rapidly heating the tube furnace to 575 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 150V/cm, wherein the preset current density is 50mA/mm 2 After keeping for 60s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing the thickness of the sintered ceramic prepared in the step five to 0.3mm by using 240-mesh abrasive paper, then polishing the front and back surfaces of the sintered ceramic to 0.2mm by using 2000-mesh abrasive paper, placing the sintered ceramic in distilled water for ultrasonic cleaning for 3min, coating silver electrode slurry on the surface of the sintered ceramic, placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic at the temperature of 600 ℃ for 10min in the air atmosphere to obtain the compact impurity-phase-free BFO-STO ceramic material.
Example 3
Step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 2 Mixing, and adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1;
step two, pouring the obtained mixed powder into a dog-bone-shaped mould with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression moulding, and demoulding the moulded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing on the blank prepared in the step two by cooling, applying pressure of 220MPa, and maintaining the pressure for 4min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on the parallel platinum wires through the two holes, connecting the other ends of the platinum wires with a power supply, and integrally placing the sample and the platinum wires in a tubular furnace;
step five, rapidly heating the tube furnace to 550 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 200V/cm, wherein the preset current density is 50mA/mm 2 Keeping for 50s, then cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing the thickness of the sintered ceramic prepared in the step five to 0.3mm by using 240-mesh abrasive paper, then polishing the front and back surfaces of the sintered ceramic to 0.2mm by using 2000-mesh abrasive paper, placing the sintered ceramic in distilled water for ultrasonic cleaning for 4min, coating silver electrode slurry on the surface of the sintered ceramic, placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic at the temperature of 590 ℃ for 15min in an air atmosphere to obtain the compact impurity-phase-free BFO-STO ceramic material.
Example 4
Step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 Mixing, and adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1;
step two, pouring the obtained mixed powder into a dog-bone-shaped mould with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression moulding, and demoulding the moulded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing forming on the blank prepared in the step two in a cold state, applying pressure of 230MPa, and keeping the pressure for 4min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on a parallel platinum wire through the two holes, connecting the other end of the platinum wire with a power supply, and integrally placing the sample and the platinum wire in a tubular furnace;
step five, rapidly heating the tube furnace to 540 ℃ at a heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 250V/cm, wherein the preset current density is 50mA/mm 2 After keeping for 60s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing the thickness of the sintered ceramic prepared in the step five to 0.3mm by using 240-mesh abrasive paper, then polishing the front side and the back side of the sintered ceramic to 0.2mm by using 2000-mesh abrasive paper, placing the sintered ceramic in distilled water for ultrasonic cleaning for 3-5 min, coating silver electrode slurry on the surface of the sintered ceramic, placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic at the temperature of 585 ℃ in an air atmosphere for 18min to obtain the compact impurity-phase-free BFO-STO ceramic material.
Example 5
Step one, according to BiFeO 3 With SrTiO 3 The mass ratio of substances is 3Taking analytically pure raw material Bi 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 Mixing, and adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1;
step two, pouring the obtained mixed powder into a dog-bone-shaped mold with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression molding, and demolding the molded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing on the blank prepared in the step two by cooling, applying pressure of 200MPa, and maintaining the pressure for 5min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on the parallel platinum wires through the two holes, connecting the other ends of the platinum wires with a power supply, and integrally placing the sample and the platinum wires in a tubular furnace;
step five, rapidly heating the tube furnace to 510 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 300V/cm, wherein the preset current density is 50mA/mm 2 After keeping for 40s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing the thickness of the sintered ceramic prepared in the step five to 0.3mm by using 240-mesh abrasive paper, then polishing the front and back surfaces of the sintered ceramic to 0.2mm by using 2000-mesh abrasive paper, placing the sintered ceramic in distilled water for ultrasonic cleaning for 3min, coating silver electrode slurry on the surface of the sintered ceramic, placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic at the temperature of 600 ℃ for 10min in the air atmosphere to obtain the compact impurity-phase-free BFO-STO ceramic material.
Comparative example 1
Step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 2 Mixing and then adding 0.1wt% MnO to the mixture 2 Mixing the raw materials, zircon and deionized water according to the mass ratio of 1Drying for 24h at the temperature of 80 ℃, and sieving by a 120-mesh sieve to obtain mixed powder with uniform size;
step two, pouring the obtained mixed powder into a dog-bone-shaped mold with the size of 20mm multiplied by 3.1mm multiplied by 1.4mm for compression molding, and demolding the molded blank to obtain a blank with a perfect shape;
step three, performing isostatic pressing on the blank prepared in the step two by cooling, applying pressure of 200MPa, and maintaining the pressure for 5min;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on the parallel platinum wires through the two holes, connecting the other ends of the platinum wires with a power supply, and integrally placing the sample and the platinum wires in a tubular furnace;
step five, rapidly heating the tube furnace to 700 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 50V/cm, wherein the preset current density is 50mA/mm 2 And after keeping for 60s, cutting off the power supply, cooling to room temperature along with the furnace, and taking out the sample, wherein the sample is not sintered.
FIG. 1 is a graph showing the variation of electric field intensity with furnace temperature during sintering at different electric field intensities; FIG. 2 is a graph showing the variation of current density with furnace temperature during sintering at different electric field strengths; it can be seen from FIGS. 1 and 2 that the BFO-STO ceramic material is not sintered at an electric field strength of 50V/cm due to insufficient energy obtained; when the voltage is more than 50V/cm, the internal conductivity of the sample is increased when the sample is at the sintering critical temperature, and the current density flowing through the sample is increased to the preset critical value (50 mA/mm) instantly 2 ) Thereby sintering occurs.
FIG. 3 is a diagram showing the relationship between the furnace temperature and the electric field; as can be seen from fig. 3, as the electric field strength increases, the start temperature required for sintering can be effectively lowered.
FIG. 4 is an XRD pattern of the products prepared in examples 2-5; as can be seen from FIG. 4, the sample obtained by firing at an electric field strength of 150V/cm exhibited a hetero-phase, whereas the other electric field strengths exhibited a single-phase perovskite structure, and no second phase was generated.
FIG. 5 is a graph of dielectric constant and dielectric loss as a function of temperature for the products prepared in examples 2-5 at different electric field strengths at a frequency of 1 MHz; as can be seen from fig. 5, it can be seen that the dielectric constant and dielectric loss of the BFO-STO ceramic do not vary much in the range of room temperature to 300 ℃ over the test temperature range, exhibiting good temperature stability, and show an increasing trend after 300 ℃, which is related to the establishment of various polarization mechanisms at high temperature, wherein the 250V/cm sintered sample maintains a lower dielectric constant and better temperature stability even within 400 ℃.
FIG. 6 is a complex impedance plot at 260 ℃ for the products prepared in examples 2-5; FIG. 6 also illustrates that a dense ceramic sample can be obtained at an electric field strength of 250V/cm.
Finally, it is to be noted that: the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and any modifications or equivalent replacements by those of ordinary skill in the art without departing from the spirit and scope of the present invention should be covered in the protection scope of the present claims.
Claims (8)
1. A preparation method of a compact impurity-free bismuth ferrite-strontium titanate ceramic material is characterized by comprising the following steps:
step one, according to BiFeO 3 With SrTiO 3 Weighing analytically pure raw material Bi according to the mass ratio of 3 2 O 3 、Fe 2 O 3 、SrCO 3 And TiO 2 Mixing, and adding 0.1wt% MnO to the mixture 2 Mixing, ball milling, drying and sieving to obtain mixed powder with uniform size;
pouring the obtained mixed powder into a dog bone-shaped mold for press molding, and demolding the molded blank to obtain a blank with an intact shape;
step three, the blank prepared in the step two is cold and is pressed and formed through isostatic pressing;
drilling holes at two ends of the blank obtained in the step three, hanging a sample on a parallel platinum wire through the two holes, connecting the other end of the platinum wire with a power supply, and integrally placing the sample and the platinum wire in a tubular furnace;
step five, rapidly heating the tube furnace to 510-620 ℃ at the heating rate of 10 ℃/min, preserving the temperature of the sample for 30min at the temperature, and applying a constant electric field of 100-300V/cm, wherein the preset current density is 50mA/mm 2 Keeping the temperature for 30-60 s, cutting off the power supply, cooling the sample to room temperature along with the furnace, and taking out the sample to obtain sintered ceramic;
and step six, polishing and cleaning the sintered ceramic prepared in the step five, coating silver electrode slurry on the surface of the sintered ceramic, then placing the sintered ceramic in a muffle furnace, and sintering the sintered ceramic for 20-30 min at 580-600 ℃ in air atmosphere to obtain the compact impurity-phase-free BFO-STO ceramic material.
2. The preparation method of the dense impurity-free bismuth ferrite-strontium titanate ceramic material of claim 1, wherein in the first step, the raw materials, zircon and deionized water are mixed according to a mass ratio of 1.
3. The method for preparing a dense impurity-free bismuth ferrite-strontium titanate ceramic material according to claim 2, wherein the first step is performed with a sieve mesh size of 120 meshes.
4. The method for preparing the dense heterogeneous bismuth ferrite-strontium titanate ceramic material according to claim 3, wherein the drying in the first step is drying at a temperature of 80 ℃ for 24h.
5. The method for preparing the compact non-hetero-phase bismuth ferrite-strontium titanate ceramic material according to claim 1, wherein the mold in the second step is a dog bone shape with a size of 20mm x 3.1mm x 1.4mm, and 0.8g of the mixed powder is weighed and poured into a grinding tool for compression molding.
6. The method for preparing the dense heterogeneous bismuth ferrite-strontium titanate ceramic material according to claim 1, wherein the pressure of the cold isostatic pressing in the third step is 200-250 MPa, and the pressure is maintained for 3-5 min.
7. The method for preparing the compact heterogeneous bismuth ferrite-strontium titanate ceramic material according to claim 1, wherein the grinding in the sixth step is to grind the sample to 0.3mm in thickness by 240-mesh sand paper, and then grind the front and back surfaces of the sample to 0.2mm in thickness by 2000-mesh sand paper.
8. The preparation method of the dense hetero-phase-free bismuth ferrite-strontium titanate ceramic material of claim 1, wherein the cleaning in the sixth step is ultrasonic cleaning in distilled water for 3-5 min.
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| CN114300269A (en) * | 2022-01-25 | 2022-04-08 | 陕西科技大学 | High-energy-storage and high-efficiency bismuth ferrite-strontium titanate ceramic and preparation method thereof |
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| US20140306381A1 (en) * | 2011-07-29 | 2014-10-16 | Rishi Raj | Methods of flash sintering |
| CN112225550A (en) * | 2020-09-11 | 2021-01-15 | 广东天瞳科技有限公司 | Piezoelectric ceramic material, preparation method thereof and piezoelectric ceramic sensor |
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
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