CN106587993B - A kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3Preparation method - Google Patents

A kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3Preparation method Download PDF

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CN106587993B
CN106587993B CN201611124371.6A CN201611124371A CN106587993B CN 106587993 B CN106587993 B CN 106587993B CN 201611124371 A CN201611124371 A CN 201611124371A CN 106587993 B CN106587993 B CN 106587993B
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汪川惠
袁松柳
王星
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Hubei University of Education
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Abstract

A kind of more iron ceramics Ba of room temperature1‑xBixTi1‑yMnyO3Preparation method, by containing barium ions, bismuth ion, titanium ion and manganese ion AB solution mix, at 80-100 DEG C of temperature, reaction obtain wet gel；Then 2-4h is dried in 150-170 DEG C of baking oven, obtains xerogel, and xerogel grinding 1-3h is obtained into powder；The powder is passed through into 500-600 DEG C of pre-burning 6-8h in Muffle furnace；It takes out powder and grinds 1-3h in air, depress to the disk that diameter is 10mm in the pressure of 10-15MPA with powder compressing machine, sintering temperature obtains double sintering Ba to 900-1000 DEG C in Muffle furnace1‑xBixTi1‑ yMnyO3Ceramics.Firstly, the bismuth ion introduced volatilizees on a small quantity at a high temperature of 900-1000 DEG C, in the case where not influencing the ferroelectric situation of barium titanate matrix, Lacking oxygen is generated in the sample；Second, the manganese ion of introducing couples to form spontaneous magnetic polaron with Lacking oxygen, so that material shows ferromagnetism.Therefore single-phase Ba is prepared using the present invention1‑xBixTi1‑yMnyO3Ceramics, discovery have ferroelectricity and ferromagnetism at room temperature, that is, have room temperature multiferroic, and ceramics dielectric constant also with higher.

Description

A kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3Preparation method
Technical field
The invention belongs to electron ceramic material technical fields, are related to a kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3's Preparation method.It in particular is a kind of being co-doped with to barium titanate matrix by Bi ion and Mn ion using collosol and gel It is modified, so that preparation has the ceramic Ba of room temperature multi-ferrum property1-xBixTi1-yMnyO3Method.
Background technique
The mutual regulation between electric polarization and magnetic moment may be implemented in magnetoelectric effect multi-iron material.This effect is possible to Break through the bottleneck of current spintronics --- the reading and control of spin states.Material with multiferroic is to generate magnetic The important sources of coupling effect.In order to realize room temperature magnetoelectric effect, and biggish magneto-electric coupled coefficient is obtained, just needed It develops with the more iron of good ferromagnetic and ferroelectric single-phase room temperature.In recent years, many single phase multi-iron materials are produced Out, such as: BiFeO3, BiMnO3, RMnO3, REMn2O5, (R: rare earth element), Ni3V2O8, delafossite CuFeO2, spinelle CoCr2O4,MnWO4, six square iron hydrochlorate (Ba, Sr) Zn2Fe12O22Etc., but most of is all that could go out at quite low temperatures Existing multiferroic.And the more iron BiFeO of the most commonly used a kind of material wherein studied, i.e. room temperature3, while there is the antiferromagnetic of room temperature And ferroelectric property, Ne&1&el temperature are 380 DEG C, ferroelectrie Curie temperature is 810 DEG C.
As most famous room temperature multi-iron material, BiFeO3 is largely had studied.Its chemical doping A are mixed The BiFeO3 of miscellaneous, B doping and AB codopes or particular configuration, such as nano particle, film etc. have related report Road.It is wherein many all with the multiferroic of room temperature, and have some with magnetocapacitance effect.Since Bi and Fe are easy in BiFeO3 In volatilization, therefore it is easy to generate miscellaneous phase during the preparation process, and the ferroelectricity of BiFeO3 material is not fine yet.Cause This, consideration manufactures room temperature multi-iron material using other approach.A kind of system with room temperature multiferroic matter is explained below.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of more iron ceramics Ba of room temperature1-xBixTi1- yMnyO3Preparation method, the ceramics be A doping high-valence state metallic elements, the single phase perovskite of B containing transition metal elements Structural material, ferroelectricity and ferromagnetism with room temperature, and there is preferable dielectricity.
The present invention provides a kind of preparation method of the more iron ceramics of room temperature,
The ceramics of perovskite structure with room temperature multiferroic matter, chemical formula Ba1-xBixTi1-yMnyO3Preparation method, Wherein 0≤x≤0.1,0≤y≤0.06.Specific preparation process is as follows:
(1) ba source compounds, titanate ester compound, bismuth source compound, manganese source compound are weighed according to stoichiometric ratio And citric acid, ba source compounds are dissolved in aqueous citric acid solution and obtain solution A, successively by titanate ester compound, bismuth Source compound and manganese source compound are dissolved in aqueous citric acid solution under ultrasonic disperse obtains solution B；
(2) solution A and B solution are uniformly mixed, it is 5-6 that ammonium hydroxide, which is added, and adjusts pH value, and it is (every to add ethylene glycol 0.01mol sample adds 10-15ml) it is used as combustion adjuvant；
(3) acquired solution is placed in 80-100 DEG C of temperature of water-bath, is chemically reacted, the reaction time is that 1-3 is small When, obtain wet gel；
(4) gained wet gel is dried into 2-4h in 150-170 DEG C of baking oven, obtains xerogel, and by xerogel in sky It is ground 1-3 hours in gas, obtains powder；
(5) by powder, first sintering temperature is 500-600 DEG C in Muffle furnace, and soaking time is 6-8 hours, takes out powder It grinds 1-3 hours in air at end；
(6) ground powder is depressed to diameter in the pressure of 10-15MPa with powder compressing machine is 10mm, with a thickness of The disk of 0.5-1mm；
(7) by the disk, second of sintering temperature is 900-1000 DEG C in Muffle furnace, and soaking time is 4-6 hours, so Afterwards in descent of temperature to taking out after 20-30 DEG C, then obtaining chemical formula is Ba1-xBixTi1-yMnyO3Room temperature more iron perovskites pottery Porcelain.
Wherein step (1) ba source compounds are barium carbonate, and titanate ester compound is butyl titanate, bismuth source chemical combination Object is bismuth nitrate, and manganese source compound is manganese acetate.
The molar ratio of metal cation and citric acid is 1:1.5 in A and B solution.
In step (2), ethylene glycol needed for every preparation 0.01mol sample is 10-15ml.
The more iron ceramics Ba of the room temperature that the present invention is prepared1-xBixTi1-yMnyO3It is single phase perovskite structure, and leads to The codope of bismuth ion and manganese ion is crossed, so that only show ferroelectric barium titanate matrix remains ferroelectricity after doping originally Property, and have ferromagnetism.For x=0.07, the sample of y=0.04, in the case where measuring electric field is 75kV/cm, Remanent polarization 2Pr is 4.0 μ C/cm2, and coercive field 2Ec is 24.8kV/cm, and remanent magnetization 2Mr is 0.0014emu/ G, coercivity 168Oe, dielectric constant is greater than 400 (when 1000Hz) at room temperature.
The present invention prepares single-phase Ba1-xBixTi1-yMnyO3 ceramics, has ferroelectricity and ferromagnetism at room temperature, that is, has Room temperature multiferroic, and ceramics dielectric constant also with higher.
Detailed description of the invention
Fig. 1 is preparation flow figure；
Fig. 2 is Ba obtained in 1-2 of the embodiment of the present invention1-xBixTi1-yMnyO3The X-ray diffractogram of ceramics；
Fig. 3 is Ba obtained in the embodiment of the present invention 11-xBixTi1-yMnyO3The scanning electron microscope (SEM) photograph of ceramics；
Fig. 4 is Ba signified in 1-2 of the embodiment of the present invention1-xBixTi1-yMnyO3The ferromagnetic property test chart of ceramics；
Fig. 5 is Ba signified in 1-2 of the embodiment of the present invention1-xBixTi1-yMnyO3The ferroelectric properties test chart of ceramics；
Fig. 6 is Ba signified in 1-2 of the embodiment of the present invention1-xBixTi1-yMnyO3The dielectric properties test chart of ceramics；
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.
Especially be illustrated, prepare reagent used in barium titanate of the present invention and be commercially available, rank be analysis it is pure or Chemistry is pure.Wherein use equipment are as follows: water-bath, high temperature sintering furnace, powder compressing machine.Test equipment are as follows: ferroelectricity analyzer, X are penetrated Line diffractometer, comprehensive property tester (PPMS), alternating temperature measurement instrument.It should be appreciated that specific embodiment described herein It is only used to explain the present invention, be not intended to limit the present invention.
Wherein, Ba obtained in Fig. 2 embodiment1-xBixTi1-yMnyO3The X-ray diffractogram of ceramics, wherein x= 0.07, y takes y=0.02, and 0.04.
Obtained Ba in Fig. 3 embodiment1-xBixTi1-yMnyO3The scanning electron microscope (SEM) photograph of ceramics, wherein x=0.07, y= 0.02。
Signified Ba in Fig. 4 embodiment1-xBixTi1-yMnyO3The ferromagnetic property test chart of ceramics, wherein x=0.07, y =0.02,0.04.
Signified Ba in Fig. 5 embodiment1-xBixTi1-yMnyO3The ferroelectric properties test chart of ceramics, wherein x=0.07, y =0.02,0.04.
Signified Ba in Fig. 6 embodiment1-xBixTi1-yMnyO3The dielectric properties test chart of ceramics, wherein x=0.07, y =0.02,0.04.
Embodiment 1:
Take raw material: analytically pure butyl titanate (Ti [OCH (CH3)2]4), five nitric hydrate bismuth (Bi (NO3)3· 5H2O), barium carbonate (BaCO3), four hydration manganese acetate ((CH3COO)3Mn·4H2O), ethylene glycol, ammonium hydroxide, monohydrate potassium (C6H8O7·H2O).According to preparation 0.02mol Ba0.93Bi0.07Ti0.98Mn0.02O3To weigh drug.
1. stoichiometrically weighing 0.0186mol (3.6707g) barium carbonate and 0.0186*1.5mol (5.8629g) one Citric acid is dissolved in 10ml deionized water by citric acid monohydrate, then weighed barium carbonate is dissolved in the aqueous solution of this citric acid In to obtaining clear solution A.
2. weigh again five water bismuth nitrate of 0.0014mol (0.6791g), 0.0196mol (6.6699g) butyl titanate, Four water acetic acid manganese of 0.0004mol (0.09804g) and 0.0214*1.5mol (6.7455g) monohydrate potassium, citric acid is molten In 20ml deionized water, then under ultrasonic wave dispersion, by weighed four fourth rouge of metatitanic acid, five nitric hydrate bismuths and four hydration vinegar Sour manganese, which is successively dissolved in the aqueous solution of this citric acid, obtains solution B.
3. solution A and B are mixed, under continuous stirring, then pH=5~6 are adjusted by adding ammonium hydroxide, form colloidal sol, then 10ml ethylene glycol is added, last resulting solution heating water bath 1-2 hours, obtains wet gel.
4. obtained wet gel is 4 hours dry at 150 DEG C, so that organic solvent is volatilized, obtain xerogel, then by gained Xerogel be ground into dry gel powder.
5. 600 DEG C pre-burning 6 hours, exclude dry gel powder in organic matter, obtain powder early period.
6. using powder compressing machine by early period pressed by powder at diameter about 1cm thickness about 0.1cm piece, at 1000 DEG C Lower firing 4h, Temperature fall further take out to room temperature, we can be obtained and measures required potsherd.
7. gained potsherd can carry out XRD, scanning electron microscope and Magnetic Measurement, and ferroelectricity and dielectric property are then needed Silver paste, and 600 DEG C of baking 20min are coated on potsherd two sides again, then available electrode, to carry out ferroelectricity and dielectric The measurement of property.
Embodiment 2:
Take raw material: analytically pure butyl titanate (Ti [OCH (CH3)2]4), five nitric hydrate bismuth (Bi (NO3)3· 5H2O), barium carbonate (BaCO3), four hydration manganese acetate ((CH3COO)3Mn·4H2O), ethylene glycol, ammonium hydroxide, monohydrate potassium (C6H8O7·H2O).According to preparation 0.02mol Ba0.93Bi0.07Ti0.96Mn0.04O3To weigh drug.
1. stoichiometrically weighing 0.0186mol (3.6707g) barium carbonate and 0.0186*1.5mol (5.8629g) one Citric acid is dissolved in 10ml deionized water by citric acid monohydrate, then weighed barium carbonate is dissolved in the aqueous solution of this citric acid In to obtaining clear solution A；
2. weigh again five water bismuth nitrate of 0.0014mol (0.6791g), 0.0192mol (6.5338g) butyl titanate, Four water acetic acid manganese of 0.0008mol (0.1961g) and 0.0214*1.5mol (6.7455g) monohydrate potassium, citric acid is dissolved in 20ml deionized water, then under ultrasonic wave dispersion, by weighed four fourth rouge of metatitanic acid, five nitric hydrate bismuths and four hydration acetic acid Manganese, which is successively dissolved in the aqueous solution of this citric acid, obtains solution B.
3. solution A and B are mixed, under continuous stirring, then pH=5~6 are adjusted by adding ammonium hydroxide, form colloidal sol, then 10ml ethylene glycol is added, last resulting solution heating water bath 1-2 hours, obtains wet gel.
4. obtained wet gel is 4 hours dry at 150 DEG C, so that organic solvent is volatilized, obtain xerogel, then by gained Xerogel be ground into dry gel powder.
5. 600 DEG C pre-burning 6 hours, exclude dry gel powder in organic matter, obtain powder early period.
6. using powder compressing machine by early period pressed by powder at diameter about 1cm thickness about 0.1cm piece, at 1000 DEG C Lower firing 4h, Temperature fall further take out to room temperature, we can be obtained and measures required potsherd.
7. gained potsherd can carry out XRD, scanning electron microscope and Magnetic Measurement, and ferroelectricity and dielectric property are then needed Silver paste, and 600 DEG C of baking 20min are coated on potsherd two sides again, then available electrode, to carry out ferroelectricity and dielectric The measurement of property.
The above is only some embodiments of the present invention, to those skilled in the art, are not departing from this hair Under the premise of bright concept, several modifications and improvements can be also carried out, these are all within the scope of protection of the present invention.

Claims (5)

1. a kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3Preparation method, which is characterized in that carried out by following step:
(1) according to stoichiometric ratio weigh ba source compounds, titanate ester compound, bismuth source compound, manganese source compound and Ba source compounds are dissolved in aqueous citric acid solution and obtain solution A by citric acid, successively by titanate ester compound, bismuth source It closes object and manganese source compound is dissolved in aqueous citric acid solution under ultrasonic disperse and obtains solution B；
(2) solution A and B solution are uniformly mixed, it is 5-6 that ammonium hydroxide, which is added, and adjusts pH value, adds ethylene glycol as combustion adjuvant；
(3) acquired solution is placed in 80-100 DEG C of temperature of water-bath, is chemically reacted, the reaction time is 1-3 hours, is obtained To wet gel；
(4) gained wet gel is dried into 2-4h in 150-170 DEG C of baking oven, obtains xerogel, and in air by xerogel 1-3h is ground, powder is obtained；
(5) by powder, first sintering temperature is 500-600 DEG C in Muffle furnace, and soaking time is 6-8 hours, takes out powder and exists It is ground 1-3 hours in air；
(6) ground powder is depressed to diameter in the pressure of 10-15MPa with powder compressing machine is 10mm, with a thickness of 0.5- The disk of 1mm；
(7) second of sintering in Muffle furnace by the disk, temperature are 900-1000 DEG C, and soaking time is 4-6 hours, are then existed For descent of temperature to taking out after 20-30 DEG C, then obtaining chemical formula is Ba1-xBixTi1-yMnyO3The more iron perovskite ceramics of room temperature；A and The molar ratio of metal cation and citric acid is 1:1.5 in B solution；Ethylene glycol needed for every preparation 0.01mol sample is 10- 15ml；Wherein the value of x is 0≤x≤0.1, and the value of y is 0≤y≤0.06.
2. preparation method described in claim 1, it is characterised in that: step (1) ba source compounds are barium carbonate, titanate esters Class compound is butyl titanate, and bismuth source compound is bismuth nitrate, and manganese source compound is manganese acetate.
3. preparation method described in claim 1, it is characterised in that: wherein B solution, which is prepared, successively will under conditions of ultrasound Four fourth rouge of metatitanic acid, bismuth nitrate and manganese acetate are dissolved in the aqueous solution of citric acid.
4. preparation method described in claim 1, it is characterised in that: disk needs nature to drop after 900-1000 DEG C of sintering Temperature further takes out furnace body to room temperature.
5. preparation method described in claim 1, it is characterised in that: the sample of x=0.07, y=0.04 are 75kV/ in electric field In the case where cm, remanent polarization 2Pr is 4.0 μ C/cm2, and coercive field 2Ec is 24.8kV/cm, remanent magnetization 2Mr For 0.0014emu/g, coercivity 168Oe, dielectric constant is greater than 400 at room temperature.
CN201611124371.6A 2016-12-08 2016-12-08 A kind of more iron ceramics Ba of room temperature1-xBixTi1-yMnyO3Preparation method Expired - Fee Related CN106587993B (en)

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