CN105645944B - A kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof - Google Patents

A kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof Download PDF

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CN105645944B
CN105645944B CN201511024110.2A CN201511024110A CN105645944B CN 105645944 B CN105645944 B CN 105645944B CN 201511024110 A CN201511024110 A CN 201511024110A CN 105645944 B CN105645944 B CN 105645944B
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蒲永平
高子岩
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof, belongs to technical field of material.The chemical composition of the composite ceramics is expressed as：(1‑x)Bi2Fe4O9‑xBaFe12O19, 0.07≤x≤0.20.The present invention is with Bi2Fe4O9For matrix, pass through compound BaFe12O19Its magnetic property is greatly improved, is multiferroic Bi2Fe4O9Practical application provide a kind of practicable method.And microwave sintering method is different from general conventional sintering, and sintering time is very short, temperature gradient is not present in sintering process, the ceramics of nano-powder sintering prepared by the method combination microwave-hydrothermal method have many advantages, such as crystallite dimension is small, and consistency is high.

Description

A kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof
Technical field
The invention belongs to technical field of material, it is related to the preparation method of multi-ferroic material, and in particular to a kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof.
Background technology
Multi-ferroic material is also known as magnetoelectric material, it refers to there is two or more basic iron (ferroelectricity, iron at the same time Magnetic and ferroelasticity) material, the research of multi-ferroic material is inseparable, same material with the research of magnetoelectric effect Middle magnetic and ferroelectricity is coexisted so that multi-ferroic material can not only make as single magnetic material and ferroelectric substance With, meanwhile, the coupling effect of magnetic and electricity in multi-ferroic material, i.e. extra electric field cause material magnetization or additional magnetic field to cause thing Occurs electric polarization inside matter so that the material has the free degree of higher in the application, is miniaturization and the multifunction of device Provide possibility.
Single-phase multi-ferroic material refer in same phase have ferroelectricity, ferromagnetism and ferroelasticity in two or more Performance.Mullite-type Bi2Fe4O9Due to causing the great research interest of people with multiferroic, magnetic and catalytic performance. It can be desirable to it is widely used in fields such as solid fuel cell, semiconductor gas sensor, spin electric devices.But Bi2Fe4O9Generally preparing BiFeO3During obtained as accessory substance.And its multiferroic is very weak, especially its magnetic property Very weak (Ms=0.082emu/g, Mr=0.001emu/g, Hc=493G), it is difficult to obtain practicality ([1] Miao Liu, Haibo Yang,Ying Lin,et al.Influence of Co doping on the magnetic properties of Bi2Fe4O9powders[J]. Journal of Materials Science:Materials in Electronics, 2014,25:4949-4953.).Bi is improved at present2Fe4O9Magnetic main method is by containing transition metal ion, is changed Whole magnetic spin structure, induced magnetization.Such as：Bi is improved by the doping of Ti ions2Fe4O9Multiferroic ([2] Z.M.Tian, Y.Qiu,S.L.Yuan,et al.Enhanced Multiferroic Properties in Ti-doped Bi2Fe4O9 Ceramics.Journal of Applied Physics,2010,108:064110.)。
However, Bi cannot significantly be improved by adulterating excessive ion2Fe4O9Magnetic property.
The content of the invention
It is an object of the invention to provide a kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof, this method behaviour Make simple, reproducible, consistency height small through composite ceramics crystallite dimension made from this method.
The present invention is to be achieved through the following technical solutions：
The invention discloses a kind of Bi2Fe4O9/BaFe12O19Composite ceramics, the chemical composition of the composite ceramics are expressed as： (1-x)Bi2Fe4O9-xBaFe12O19, 0.07≤x≤0.20.
The invention also discloses a kind of Bi2Fe4O9/BaFe12O19The preparation method of composite ceramics, comprises the following steps：
1) 1 is pressed:2~3 molar ratio, takes Bi (NO3)3·5H2O and Fe (NO3)3·9H2O, be dissolved in concentration for 4~ In the salpeter solution of 5mol/L；
2) 1g is pressed：The solid-liquid ratio of 4~5mL, KOH is dissolved in distilled water, and KOH solution is made；
3) solution made from step 1) is instilled in KOH solution made from step 2), mixed solution is made, by mixed solution At 180~220 DEG C, microwave hydrothermal reacts 25~35min, and reaction product is made, reaction product is washed to neutrality；
4) 1 is pressed:8~12 molar ratio, takes Ba (NO3)2With Fe (NO3)3·9H2O, is dissolved in distilled water, adjusts solution To >=13 alkaline solution is made, by the alkaline solution at 170~190 DEG C, 25~30min of microwave hydrothermal, is made reaction in pH value Thing, neutrality is washed till by reactants water；
5) dried after product made from step 3) and step 4) is mixed, obtain mixed powder, adding volumetric concentration is 5% PVA binding agents, are then granulated, are compressing, and wafer type base substrate is made；
6) wafer type base substrate is obtained into ceramic green, then by ceramic green at 800 DEG C~850 DEG C in 600 DEG C of dumping 2h 1~5min of lower microwave sintering, is made composite ceramics.
After composite ceramics is made in step 6), then surface polishing is carried out to it, by silver electrode, keep the temperature 10min at 600 DEG C, burn Silver electrode is oozed, obtains composite ceramics sample.
The temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with 3 DEG C/heating rate of min is warming up to 500 DEG C from 200 DEG C, 600 DEG C finally are warming up to from 500 DEG C with the programming rate of 5 DEG C/min, During cooling, furnace cooling.
The temperature increasing schedule of the step 6) dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then 500 DEG C are warming up to from 200 DEG C with the heating rate of 3 DEG C/min, is finally warming up to 600 from 500 DEG C with the programming rate of 5 DEG C/min DEG C, during cooling, furnace cooling.
The output power of the step 6) microwave sintering is 1400W, and heating rate is 25 DEG C/min, and in 30min from Room temperature is to 800 DEG C~850 DEG C, during cooling, furnace cooling.
Step 3) and step 4) water scouring water are distilled water, are washed 5~6 times.
Raw material Bi (NO3)3·5H2O、Fe(NO3)3·9H2O, KOH and Ba (NO3)2Purity be more than 99.0%.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention uses BaFe12O19Modified Bi2Fe4O9The method of magnetic ceramics, advantage are notable：
1) powder is prepared using microwave-hydrothermal method, has crystal grain small, size uniform, crystallinity is high, and the reaction time is short etc. excellent Point；
2) using microwave sintering method sintering ceramics, different from general conventional sintering, sintering time is short, in sintering process not There are temperature gradient, the volatilization problems of Bi elements are efficiently solved, nano-powder prepared by the method combination microwave-hydrothermal method is burnt The ceramics of knot have many advantages, such as crystallite dimension is small, and consistency is high；
3) with Bi (NO3)3·5H2O, Ba (NO3)2With Fe (NO3)3·9H2O is raw material, and raw material is simple.
The BaFe prepared through the method for the present invention12O19Modified Bi2Fe4O9Magnetic ceramics substantially increases multiferroic Bi2Fe4O9 Magnetic property, have crystal grain small, be multiferroic Bi the advantages that size uniform, crystallinity is high2Fe4O9Practical application provide one The practicable method of kind.
Brief description of the drawings
Fig. 1 is BaFe12O19Modified Bi2Fe4O9The XRD spectrum of magnetic ceramic material；
Fig. 2 is BaFe12O19Modified Bi2Fe4O9The EDS photos of magnetic ceramic material；
Fig. 3 is BaFe12O19Modified Bi2Fe4O9The SEM photograph of magnetic ceramic material；
Wherein, (a), (b), (c), (d), (e), (f) are respectively x=0.07,0.08,0.10,0.12,0.15 and 0.20 Composite ceramics；
Fig. 4 is BaFe12O19Modified Bi2Fe4O9The ferroelectric hysteresis loop of magnetic ceramic material；
Fig. 5 is BaFe12O19Modified Bi2Fe4O9The hysteresis curve of magnetic ceramic material.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Embodiment 1
Composite ceramics (1-x) Bi in the present embodiment2Fe4O9-xBaFe12O19Middle x=0.07, preparation method include following step Suddenly：
1) according to 1:2 molar ratio weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.212g3)3·9H2O, it is molten Solution is in the salpeter solution that 5ml concentration is 5mol/L；
2) KOH of 25g is weighed, is dissolved in 20mL distilled water, KOH solution is made；
3) solution made from step 1) is instilled in KOH solution made from step 2) dropwise, obtains mixed solution；Will mixing Solution is transferred in water heating kettle, and 200 DEG C of microwave hydrothermal 30min obtain reaction product；Reaction product is washed 5~6 times to neutrality；
4) according to 1：8 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 3.8784g3)3·9H2O, dissolving In 40ml distilled water；The KOH solution of 4mol/L is added dropwise, adjusts solution ph to 13, obtained alkaline solution is molten by the alkalescence Liquid is transferred in water heating kettle, and reaction product is obtained within 30 minutes in 180 DEG C of microwave hydrothermals, and reaction product is washed 5~6 times into Property；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.07), and drying is mixed Powder, adds the PVA bonding agents that volumetric concentration is 5%, is granulated, is dry-pressing formed, obtains a diameter of 10mm, and thickness is 1mm's Disc base substrate；
6) disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, then by ceramic green in 820 DEG C of microwaves Sintering obtains composite ceramics in 5 minutes；
Wherein, the temperature increasing schedule of dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with 3 DEG C/ The heating rate of min is warming up to 500 DEG C from 200 DEG C, 600 DEG C is finally warming up to from 500 DEG C with the programming rate of 5 DEG C/min, drop Wen Shi, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 800 DEG C~850 DEG C, during cooling, furnace cooling；
7) composite ceramics surface is polished, by silver electrode, 10 minutes is kept the temperature at 600 DEG C, burning infiltration silver electrode, finally obtains multiple Close ceramics sample.Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, Then 500 DEG C are warming up to from 200 DEG C with the heating rate of 3 DEG C/min, are finally heated up with the programming rate of 5 DEG C/min from 500 DEG C To 600 DEG C, during cooling, furnace cooling.
Embodiment 2
Composite ceramics (1-x) Bi in the present embodiment2Fe4O9-xBaFe12O19Middle x=0.08, preparation method include following step Suddenly：
1)：According to 1:3 molar ratio weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.818g3)3·9H2O, It is dissolved in the salpeter solution that 5ml concentration is 5mol/L；
2) KOH of 25g is weighed, is dissolved in 20mL distilled water, KOH solution is made；
3) solution obtained by step 1) is instilled in the KOH solution obtained by step 2) dropwise, obtains mixed solution, will mixed Solution is transferred in water heating kettle, and 200 DEG C of microwave hydrothermals obtain reaction product in 30 minutes, and reaction product is washed 5~6 times into Property；
4) according to 1：8 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 3.8784g3)3·9H2O, dissolving In 40ml distilled water, the KOH solution of 4mol/L is added dropwise, adjusts solution ph to 13, alkaline solution is made, by alkaline solution It is transferred in water heating kettle, reaction product is obtained within 30 minutes in 180 DEG C of microwave hydrothermals, reaction product is washed 5~6 times to neutrality；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.08), and drying is mixed Powder, adds the PVA bonding agents that volumetric concentration is 5%, is granulated, is dry-pressing formed, obtains a diameter of 10mm, and thickness is 1mm's Disc base substrate；
6) disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, then by ceramic green, 820 DEG C of microwaves Sintering obtains composite ceramics in 5 minutes；
Wherein, the temperature increasing schedule of dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with 3 DEG C/ The heating rate of min is warming up to 500 DEG C from 200 DEG C, 600 DEG C is finally warming up to from 500 DEG C with the programming rate of 5 DEG C/min, drop Wen Shi, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 800 DEG C~850 DEG C, during cooling, furnace cooling；
7) composite ceramics surface is polished, by silver electrode, 10 minutes is kept the temperature at 600 DEG C, burning infiltration silver electrode, finally obtains multiple Close ceramics sample.Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, Then 500 DEG C are warming up to from 200 DEG C with the heating rate of 3 DEG C/min, are finally heated up with the programming rate of 5 DEG C/min from 500 DEG C To 600 DEG C, during cooling, furnace cooling.
Embodiment 3
Composite ceramics (1-x) Bi in this example2Fe4O9-xBaFe12O19Middle x=0.10, preparation method comprise the following steps：
1) according to 1:2 molar ratio weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.212g3)3·9H2O, it is molten Solution is in the salpeter solution that 5ml concentration is 4mol/L；
2) KOH of 25g is weighed, is dissolved in 25mL distilled water, KOH solution is made；
3) solution obtained by step 1) is instilled in the KOH solution obtained by step 2) dropwise, obtains mixed solution, will mixed Solution is transferred in water heating kettle, and 180 DEG C of microwave hydrothermals obtain reaction product in 35 minutes, and reaction product is washed 5~6 times into Property；
4) according to 1:9 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 4.3632g3)3·9H2O, dissolving In 40ml distilled water, the KOH solution of 4mol/L is added dropwise, adjusts solution ph to 14, alkaline solution is made, alkaline solution is turned Move in water heating kettle, reaction product is obtained within 30 minutes in 170 DEG C of microwave hydrothermals, reaction product is washed 5~6 times to neutrality；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.10), and drying is mixed Powder；The PVA bonding agents that volumetric concentration is 5% are added, is granulated, is dry-pressing formed, obtain a diameter of 10mm, thickness is 1mm's Disc base substrate；
6) obtained disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, ceramic green is micro- at 820 DEG C Ripple sinters 3 minutes and obtains composite ceramics；
Wherein, the temperature increasing schedule of the dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with The heating rate of 3 DEG C/min is warming up to 500 DEG C from 200 DEG C, is finally warming up to 600 from 500 DEG C with the programming rate of 5 DEG C/min DEG C, during cooling, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 820 DEG C, during cooling, furnace cooling；
7) the composite ceramics surface for obtaining step 6) polishes, and by silver electrode, 10 minutes are kept the temperature at 600 DEG C, burning infiltration silver electricity Pole, finally obtains composite ceramics sample.Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature 200 DEG C are warming up to, is then warming up to 500 DEG C from 200 DEG C with the heating rate of 3 DEG C/min, finally with the heating speed of 5 DEG C/min Degree is warming up to 600 DEG C from 500 DEG C, during cooling, furnace cooling.
Embodiment 4
Composite ceramics (1-x) Bi in this example2Fe4O9-xBaFe12O19Middle x=0.12, preparation method comprise the following steps：
1) according to 1:2 molar ratio, weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.212g3)3·9H2O, It is dissolved in the salpeter solution that 5ml concentration is 5mol/L；
2) KOH of 25g is weighed, is dissolved in 20mL distilled water, KOH solution is made；
3) solution obtained by step 1) is instilled in the KOH solution obtained by step 2) dropwise, obtains mixed solution, will mixed Solution is transferred in water heating kettle, and 220 DEG C of microwave hydrothermals obtain reaction product in 25 minutes；Reaction product is washed 5-6 times to neutrality；
4) according to 1:10 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 4.848g3)3·9H2O, dissolving In 40ml distilled water, the KOH solution of 4mol/L is added dropwise, adjusts solution ph to 13, obtained alkaline solution is molten by the alkalescence Liquid is transferred in water heating kettle, and reaction product is obtained within 25 minutes in 190 DEG C of microwave hydrothermals, and reaction product is washed 5~6 times into Property；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.12), and drying is mixed Powder, adds 5% PVA bonding agents, is granulated, is dry-pressing formed, obtains a diameter of 10mm, and thickness is the disc base of 1mm Body；
6) disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, by ceramic green, 850 DEG C of microwave sinterings 1 Minute obtains composite ceramics；
Wherein, the temperature increasing schedule of the dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with The heating rate of 3 DEG C/min is warming up to 500 DEG C from 200 DEG C, is finally warming up to 600 from 500 DEG C with the programming rate of 5 DEG C/min DEG C, during cooling, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 850 DEG C, during cooling, furnace cooling；
7) the composite ceramics surface for obtaining step 6) polishes, and by silver electrode, 10 minutes are kept the temperature at 600 DEG C, burning infiltration silver electricity Pole, finally obtains composite ceramics sample.Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature 200 DEG C are warming up to, is then warming up to 500 DEG C from 200 DEG C with the heating rate of 3 DEG C/min, finally with the heating speed of 5 DEG C/min Degree is warming up to 600 DEG C from 500 DEG C, during cooling, furnace cooling.
Embodiment 5
Composite ceramics (1-x) Bi in this example2Fe4O9-xBaFe12O19Middle x=0.15, preparation method comprise the following steps：
1) according to 1:2 molar ratio weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.212g3)3·9H2O, it is molten Solution is in the salpeter solution that 5ml concentration is 5mol/L；
2) KOH of 25g is weighed, is dissolved in 20mL distilled water, KOH solution is made；
3) solution obtained by step 1) is instilled in the KOH solution obtained by step 2) dropwise, obtains mixed solution, by step 3) mixed solution obtained by is transferred in water heating kettle, and 180 DEG C of microwave hydrothermals obtain reaction product in 35 minutes, and reaction product is washed 5~6 times extremely neutral；
4) according to 1:11 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 5.3328g3)3·9H2O, dissolving In 40ml distilled water, the KOH solution of 4mol/L is added dropwise, adjusts solution ph to 13, obtained alkaline solution is molten by the alkalescence Liquid is transferred in water heating kettle, and reaction product is obtained within 30 minutes in 170 DEG C of microwave hydrothermals, and reaction product is washed 5-6 times to neutrality；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.15), and drying is mixed Powder, 5% PVA bonding agents are added in mixed powder, is granulated, is dry-pressing formed, obtain a diameter of 10mm, and thickness is 1mm's Disc base substrate；
6) disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, then by ceramic green, 800 DEG C of microwaves Sintering obtains composite ceramics in 5 minutes；
The temperature increasing schedule of the dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with 3 DEG C/ The heating rate of min is warming up to 500 DEG C from 200 DEG C, 600 DEG C is finally warming up to from 500 DEG C with the programming rate of 5 DEG C/min, drop Wen Shi, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 800 DEG C, during cooling, furnace cooling；
7) composite ceramics surface is polished, by silver electrode, 10 minutes is kept the temperature at 600 DEG C, burning infiltration silver electrode, finally obtains multiple Close ceramics sample；Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, Then 500 DEG C are warming up to from 200 DEG C with the heating rate of 3 DEG C/min, are finally heated up with the programming rate of 5 DEG C/min from 500 DEG C To 600 DEG C, during cooling, furnace cooling.
Embodiment 6
Composite ceramics (1-x) Bi in the present embodiment2Fe4O9-xBaFe12O19Middle x=0.20, preparation method include following step Suddenly：
1) according to 1:2 molar ratio, weighs the Bi (NO of 0.728g3)3·5H2Fe (the NO of O and 1.212g3)3·9H2O, It is dissolved in the salpeter solution that 5ml concentration is 5mol/L；
2) KOH of 25g is weighed, is dissolved in 20mL distilled water, KOH solution is made；
3) solution obtained by step 1) is instilled in the KOH solution obtained by step 2) dropwise, obtains mixed solution, will mixed Solution is transferred in water heating kettle, and 200 DEG C of microwave hydrothermals obtain reaction product in 30 minutes, and reaction product is washed 5-6 times to neutrality；
4) according to 1:12 molar ratio, weighs the Ba (NO of 0.3136g3)2With the Fe (NO of 5.8176g3)3·9H2O, dissolving In 40ml distilled water, the KOH solution of 4mol/L is added dropwise, adjusts solution ph to 13, obtained alkaline solution is molten by the alkalescence Liquid is transferred in water heating kettle, and reaction product is obtained within 30 minutes in 180 DEG C of microwave hydrothermals, and reaction product is washed 5-6 times to neutrality；
5) product for obtaining step 3) and step 4) is mixed (with the mixed in molar ratio of x=0.20), and drying is mixed Powder, adds 5% PVA bonding agents, is granulated, is dry-pressing formed, obtains a diameter of 10mm, and thickness is the disc base of 1mm Body；
6) disc base substrate is obtained into ceramic green when 600 DEG C of dumpings 2 are small, by ceramic green in 820 DEG C of microwave sinterings 5 Minute obtains composite ceramics；
The temperature increasing schedule of the dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with 3 DEG C/ The heating rate of min is warming up to 500 DEG C from 200 DEG C, 600 DEG C is finally warming up to from 500 DEG C with the programming rate of 5 DEG C/min, drop Wen Shi, furnace cooling；
The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature liter in 30min Temperature is to 820 DEG C, during cooling, furnace cooling；
7) obtained composite ceramics surface is polished, by silver electrode, 10 minutes is kept the temperature at 600 DEG C, burning infiltration silver electrode, finally Obtain composite ceramics sample.Wherein, the temperature increasing schedule of burning infiltration silver electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, 500 DEG C then are warming up to from 200 DEG C with the heating rate of 3 DEG C/min, finally with the programming rate of 5 DEG C/min from 500 DEG C it is warming up to 600 DEG C, during cooling, furnace cooling
Fig. 1 and Fig. 2 is referred to, implements (1-x) Bi prepared by above example2Fe4O9-xBaFe12O19Composite ceramic material XRD spectrum and EDS analysis photo in as can be seen that above example in synthesized Bi2Fe4O9And BaFe12O19Mutually altogether The composite ceramics deposited.At the same time, it can be seen that exist without other dephasigns, and this two-phase crystallinity is higher, without interreaction, changes It is preferable to learn compatibility.From figure 3, it can be seen that obtained composite ceramics is by micron-sized Bi2Fe4O9Grain matrix and nano level Magnetic enhancement phase BaFe12O19Crystal grain is formed.Referring to Fig. 4, the ferroelectric hysteresis loop for the composite ceramics being prepared for embodiment 5 can be with Find out addition magnetic enhancement phase BaFe12O19, do not weaken Bi2Fe4O9The ferroelectricity of matrix.Referring to Fig. 5, it can be seen that with Magnetic enhancement phase BaFe12O19Gradual increase, the ferromagnetism of composite ceramics greatly enhances.And calculate its hysteresis curve Rectangular degree (R=Mr/Ms), it is found that the rectangular degree of all embodiments is both greater than 0.5.Usually the material with larger rectangular degree is wide It is general to be suitable for field (E.C.Stoner, E.P.Wohlfarth.A the Mechanism of such as Magnetic Memory storage medium Magnetic Hysteresis in Heterogeneous Alloys.Philosophical Transactions of the Royal Society London A, 1948,240:599-642.).Table 1 compared for the master of the present invention and other achievements in research Magnetic parameter is wanted, the magnetic property tool of material prepared by the present invention is greatly improved.
Table 1
[1]Jiadong Zang,Wook Jo,Haibo Zhang,Bi1/2Na1/2TiO3–BaTiO3Based Thick- film Capacitors for High-temperature Applications Journal of the European Ceramic Society,2014,34:37–43.
[2]M.A.Ahmed,S.F.Mansour,H.Ismael.A Comparative Study on the Magnetic and Electrical Properties of MFe12O19(M=Ba and Sr)/BiFeO3Nanocomposites.Journ al of Magnetism and Magnetic Materials,2015,378:376–388.
[3]R.Asih,M.Gufron,T.Amrillah,Effect of Pb Doping on Multiphase Coexistence and Magneto-electric Properties of Bismuth Ferrite.AIP Conference Proceedings,2014,1591: 1339-1341.
[4]Y.Qiu,Z.J.Zou,R.R.Sang,et al.Enhanced Magnetic and Ferroelectric Properties in Cr Doped Bi2Fe4O9Ceramics.Journal of Materials Science:Materials in Electronics,2015, 26:1732-1736.
[5]Dimple P.Dutta,C.Sudakar,Pavana S.V.Mocherla,et al.Enhanced Magnetic and Ferroelectric Properties in Scandium Doped Nano Bi2Fe4O9.Materials Chemistry and Physics,2012, 135:998-1004.
[6]Miao Liu,Haibo Yang,Ying Lin,et al.Influence of Co doping on the magnetic properties of Bi2Fe4O9powders.Journal of Materials Science:Materials in Electronics,2014, 25:4949-4953.
[7]Z.M.Tian,Y.Qiu,S.L.Yuan,et al.Enhanced Multiferroic Properties in Ti-doped Bi2Fe4O9 Ceramics.Journal of Applied Physics,2010,108:064110.
[8]Ying Lin,Pan Kang,Haibo Yang,et al.Preparation and Magnetic Properties of Bi2Fe4O9/CoFe2O4Composite Powders.Journal of Materials Science: Materials in Electronics, 2015,26(2):1102-1106.
In conclusion the present invention is prepared for Bi by microwave-hydrothermal method and microwave sintering method2Fe4O9/ BaFe12O19It is compound Ceramics.With Bi2Fe4O9For matrix, pass through compound BaFe12O19Its magnetic property is greatly improved, is multiferroic Bi2Fe4O9Reality Border application provides a kind of practicable method.And microwave sintering method is different from general conventional sintering, and sintering time is very It is short, temperature gradient is not present in sintering process, the ceramics of nano-powder sintering prepared by the method combination microwave-hydrothermal method have Many advantages, such as crystallite dimension is small, and consistency is high, is multiferroic Bi2Fe4O9Practical application provide a kind of practicable side Method.
It is disclosed by the invention to use BaFe12O19Modified Bi2Fe4O9Magnetic ceramics and preparation method thereof is likely to become preparation Bismuth ferrite multi-ferroic material technically and financially and excellent new way, more preferable magnetic property can be obtained by compound.Six Angle barium ferrite BaFe12O19It is a kind of ferromagnetic oxides, and his dielectric and magnetic property allow to answer in power frequency and microwave frequency With.Especially higher resistivity, relatively low magnetic loss and less dielectric loss can be used as microwave device and magnetic device To use.

Claims (8)

  1. A kind of 1. Bi2Fe4O9/BaFe12O19Composite ceramics, it is characterised in that the chemical composition of the composite ceramics is expressed as：(1-x) Bi2Fe4O9-xBaFe12O19, 0.07≤x≤0.20；The composite ceramics is made by following methods：
    1) 1 is pressed:2~3 molar ratio, takes Bi (NO3)3·5H2O and Fe (NO3)3·9H2O, it is 4~5mol/L's to be dissolved in concentration In salpeter solution；
    2) 1g is pressed：The solid-liquid ratio of 0.8~1mL, KOH is dissolved in distilled water, and KOH solution is made；
    3) solution made from step 1) is instilled in KOH solution made from step 2), mixed solution is made, mixed solution is existed At 180~220 DEG C, microwave hydrothermal reacts 25~35min, and reaction product is made, reaction product is washed to neutrality；
    4) 1 is pressed:8~12 molar ratio, takes Ba (NO3)2With Fe (NO3)3·9H2O, is dissolved in distilled water, adjusts solution ph Extremely >=13, alkaline solution is made, by the alkaline solution at 170~190 DEG C, 25~30min of microwave hydrothermal, is made reactant, Reactants water is washed till neutrality；
    5) dried after product made from step 3) and step 4) is mixed, obtain mixed powder, it is 5% to add volumetric concentration PVA binding agents, are then granulated, are compressing, and base substrate is made；
    6) base substrate is obtained into ceramic green in 600 DEG C of dumping 2h, then by ceramic green at 800 DEG C~850 DEG C microwave sintering 1~5min, is made composite ceramics.
  2. A kind of 2. Bi2Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that comprise the following steps：
    1) 1 is pressed:2~3 molar ratio, takes Bi (NO3)3·5H2O and Fe (NO3)3·9H2O, it is 4~5mol/L's to be dissolved in concentration In salpeter solution；
    2) 1g is pressed：The solid-liquid ratio of 0.8~1mL, KOH is dissolved in distilled water, and KOH solution is made；
    3) solution made from step 1) is instilled in KOH solution made from step 2), mixed solution is made, mixed solution is existed At 180~220 DEG C, microwave hydrothermal reacts 25~35min, and reaction product is made, reaction product is washed to neutrality；
    4) 1 is pressed:8~12 molar ratio, takes Ba (NO3)2With Fe (NO3)3·9H2O, is dissolved in distilled water, adjusts solution ph Extremely >=13, alkaline solution is made, by the alkaline solution at 170~190 DEG C, 25~30min of microwave hydrothermal, is made reactant, Reactants water is washed till neutrality；
    5) dried after product made from step 3) and step 4) is mixed, obtain mixed powder, it is 5% to add volumetric concentration PVA binding agents, are then granulated, are compressing, and base substrate is made；
    6) base substrate is obtained into ceramic green in 600 DEG C of dumping 2h, then by ceramic green at 800 DEG C~850 DEG C microwave sintering 1~5min, is made composite ceramics.
  3. 3. Bi according to claim 22Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that step 6) After composite ceramics is made, then surface polishing is carried out to it, by silver electrode, 10min is kept the temperature at 600 DEG C, burning infiltration silver electrode, is made To composite ceramics sample.
  4. 4. Bi according to claim 32Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that burning infiltration silver The temperature increasing schedule of electrode is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with the heating rate of 3 DEG C/min 500 DEG C are warming up to from 200 DEG C, is finally warming up to 600 DEG C from 500 DEG C with the programming rate of 5 DEG C/min, during cooling, furnace cooling.
  5. 5. Bi according to claim 22Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that step 6) The temperature increasing schedule of the dumping is：With the heating rate of 2 DEG C/min from room temperature to 200 DEG C, then with the heating of 3 DEG C/min Speed is warming up to 500 DEG C from 200 DEG C, is finally warming up to 600 DEG C from 500 DEG C with the programming rate of 5 DEG C/min, during cooling, with stove Cooling.
  6. 6. Bi according to claim 22Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that step 6) The output power of the microwave sintering is 1400W, and heating rate is 25 DEG C/min, and from room temperature to 800 DEG C in 30min ~850 DEG C, during cooling, furnace cooling.
  7. 7. Bi according to claim 22Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that step 3) It is distilled water with step 4) water scouring water, washes 5~6 times.
  8. 8. Bi according to claim 22Fe4O9/BaFe12O19The preparation method of composite ceramics, it is characterised in that raw material Bi (NO3)3·5H2O、Fe(NO3)3·9H2O, KOH and Ba (NO3)2Purity be more than 99.0%.
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