CN104177076B - A kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof - Google Patents

A kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof Download PDF

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CN104177076B
CN104177076B CN201410399506.4A CN201410399506A CN104177076B CN 104177076 B CN104177076 B CN 104177076B CN 201410399506 A CN201410399506 A CN 201410399506A CN 104177076 B CN104177076 B CN 104177076B
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citric acid
stupalith
doping
multiferroic
iron
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CN104177076A (en
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袁松柳
黄帅
孙海根
时丽然
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Huazhong University of Science and Technology
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Abstract

The present invention relates to a kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof, the method adopts citric acid-nitrate sol-gel method, and by pyroprocessing, obtaining molecular formula prepared by the present invention is Bi 2fe 4-xal xo 9the multiferroic stupalith of (x=0,0.2,0.4,0.6).This stupalith possesses phase structure and room temperature multiferroic, and by changing Al 3+doping can regulate room temperature magnetism and the ferroelectricity of material.Preparation technology of the present invention is simple, and sinter phase temperature into low, sintering time is short, and cost is low, and without the need to reducing atmosphere, environment-protecting asepsis is pollution-free.

Description

A kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof
Technical field
The present invention relates to multiferroic technical field of ceramic material, be specifically related to a kind of non-magnetic metal ion A l 3+doping Bi 2fe 4o 9room temperature multiferroic stupalith and preparation method thereof.
Background technology
Multi-ferroic material refers to that ferroelectric, ferromagnetic and iron bullet coexists in order and has the material of magnetoelectricity/bullet coupling character at a certain temperature, interaction between this multiple S order parameter compensate for that pure (instead) is ferroelectric, (instead) is ferromagnetic or the deficiency of iron bullet material, and the design for multifunction electronic information recording device of future generation provides an extra degree of freedom.Simultaneously, the magnetoelectric effect of multi-ferroic material is different from other magneto-electric coupled material part and is, except external field evoked magnetoelectric effect, also show spontaneous magnetoelectric effect, make change the magnetic of multiferroic by electric field or change its electrical property by magnetic field and become possibility.This magnetic and intercoupling of electricity have wide application prospect at high-technology fields such as information storage, Magnetic Sensor, spin electric device, unicircuit, have become international study hotspot.
Up to now, BiFeO 3as the typical single-phase room temperature multi-iron material of one, studied widely.But, single-phase BiFeO 3synthesis relatively difficult, often along with other dephasigns in product.Due to the huge applications prospect of room temperature multi-iron material, still need to find more single-phase room temperature multi-iron material.Recently, another bismuthino ferriferous oxide Bi 2fe 4o 9being reported in 250K and there is ferroelectric transformation, there is antiferromagnetic transition in 260K, and baffles due to the spin under low temperature, there is antiferromagnetic and ferroelectric coupling effect simultaneously.Although Bi 2fe 4o 9ferroelectric and antiferromagnetic transition temperature a little less than room temperature, but replace A position or B position atom by chemical element part, at room temperature still can obtain weak ferromegnetism and ferroelectricity simultaneously.In addition, single-phase Bi 2fe 4o 9than being easier to synthesis.At present, the Al adopting citric acid-nitrate sol-gel method to prepare 3+doping Bi 2fe 4o 9multiferroic stupalith is still without any report.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of Al 3+doping Bi 2fe 4o 9multiferroic stupalith and preparation method thereof, the stupalith that this preparation method obtains possesses room temperature many iron characteristic.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) under room temperature, first prepare citric acid solution, load weighted citric acid is put into beaker, adds distilled water, dissolve under magnetic stirring, form clear solution; Then analytically pure Bismuth trinitrate, iron nitrate, aluminum nitrate is added, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned three kinds of metallic cations is 1:1 ~ 1.5:1, and citric acid is as complexing agent, Bismuth trinitrate, iron nitrate, aluminum nitrate are as metallic cation source, the mol ratio of described Bismuth trinitrate, iron nitrate, aluminum nitrate is 2:(4-x): x, x=(0,0.2,0.4,0.6);
(2) when constantly stirring, be 7 ~ 8 by ammoniacal liquor adjust ph, mixing solutions ageing 12 ~ 24 hours; Then in a water bath 80 DEG C ~ 100 DEG C by solution evaporate to dryness removing moisture, 150 DEG C in an oven ~ 170 DEG C dryings, until form black xerogel;
(3) xerogel collected fully is ground, 500 DEG C in atmosphere ~ 600 DEG C thermal treatment 4 ~ 6 hours, get rid of organism, obtain precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 4-xal xo 9ceramics sample.
Described Al 3+doping Bi 2fe 4-xal xo 9the Bi that the preparation method of many iron stupalith obtains 2fe 4-xal xo 9many iron stupalith, has structure single-phase and room temperature many iron characteristic, wherein x=(0,0.2,0.4,0.6).
The present invention has the following advantages:
The Bi that the present invention prepares 2fe 4-xal xo 9many iron stupalith has the single-phase and room temperature multiferroic of structure, and can by changing Al 3+doping thus the magnetic of controlled material and ferroelectricity, be the multifunctional ceramic material that a class has broad prospect of application.
Preparation method of the present invention compared with traditional solid reaction process, pottery to sinter phase temperature into low, sintering time is short, and preparation technology is simple, with low cost, environment-protecting asepsis, is a kind of well low-temp ceramics sintering process.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is further described in detail.
Fig. 1 is different al in embodiment 1 to embodiment 4 3+doping Bi 2fe 4o 9the XRD figure spectrum of ceramics sample, corresponding x=0,0.2,0.4,0.6 respectively.
Fig. 2 is different al in embodiment 1 to embodiment 4 3+doping Bi 2fe 4o 9the room temperature magnetic hysteresis loop of ceramics sample; X=0,0.2,0.4,0.6, respectively corresponding diagram 2 (a), Fig. 2 (b), Fig. 2 (c), Fig. 2 (d).
Fig. 3 is different al in embodiment 1 to embodiment 4 3+doping Bi 2fe 4o 9the room temperature ferroelectric hysteresis loop of ceramics sample; X=0,0.2,0.4,0.6, respectively corresponding diagram 3 (a), Fig. 3 (b), Fig. 3 (c), Fig. 3 (d).
Embodiment
Embodiment 1
Utilize citric acid-nitrate sol-gel method, preparation Bi 2fe 4-xal xo 9(x=0) multiferroic pottery.The first step, take the beaker that 0.06mol citric acid puts into 100mL, add distilled water 20mL, dissolve under magnetic stirring, form clear solution, then take 0.02mol Bismuth trinitrate, 0.04mol iron nitrate successively, and add in above-mentioned citric acid solution, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned two kinds of metallic cations is 1:1.Second step, when constantly stirring, is 7 by ammoniacal liquor adjust ph, mixing solutions ageing 12 hours; Then in a water bath 80 DEG C by the removing of solution evaporate to dryness moisture, in an oven 150 DEG C of dryings, until form black xerogel.3rd step, fully grinds the xerogel collected, in atmosphere 500 DEG C of thermal treatment 6 hours, gets rid of organism, obtains precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 4o 9ceramics sample.
Utilize the Bi that embodiment 1 prepares 2fe 4o 9the XRD of multiferroic ceramics sample as shown in Figure 1, observes all diffraction peaks and the Bi of orthohormbic structure from Fig. 1 2fe 4o 9coincide, show single-phase, the diffraction peak without second-phase occurs.Fig. 2, Fig. 3 sets forth Bi 2fe 4o 9magnetic hysteresis loop, ferroelectric hysteresis loop.Wherein, the curve x=0 that represents in Fig. 1, Fig. 2, Fig. 3 of example 1.
Embodiment 2
Utilize citric acid-nitrate sol-gel method, preparation Bi 2fe 4-xal xo 9(x=0.2) multiferroic pottery.The first step, take the beaker that 0.072mol citric acid puts into 100mL, add distilled water 20mL, dissolve under magnetic stirring, form clear solution, then take 0.02mol Bismuth trinitrate, 0.038mol iron nitrate, 0.002mol aluminum nitrate successively, and add in above-mentioned citric acid solution, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned three kinds of metallic cations is 1.2:1.Second step, when constantly stirring, is 7 by ammoniacal liquor adjust ph, mixing solutions ageing 18 hours; Then in a water bath 90 DEG C by the removing of solution evaporate to dryness moisture, in an oven 160 DEG C of dryings, until form black xerogel.3rd step, fully grinds the xerogel collected, in atmosphere 550 DEG C of thermal treatment 5 hours, gets rid of organism, obtains precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 3.8al 0.2o 9ceramics sample.
Utilize the Bi that embodiment 2 prepares 2fe 3.8al 0.2o 9the XRD of multiferroic ceramics sample as shown in Figure 1, observes all diffraction peaks and the Bi of orthohormbic structure from Fig. 1 2fe 4o 9coincide, show single-phase, the diffraction peak without second-phase occurs, shows Al 3+fe can be replaced completely 3+enter into Bi 2fe 4o 9lattice in go.Fig. 2, Fig. 3 sets forth Bi 2fe 3.8al 0.2o 9magnetic hysteresis loop, ferroelectric hysteresis loop.Wherein, the curve x=0.2 that represents in Fig. 1, Fig. 2, Fig. 3 of example 2.
Embodiment 3
Utilize citric acid-nitrate sol-gel method, preparation Bi 2fe 4-xal xo 9(x=0.4) multiferroic pottery.The first step, take the beaker that 0.078mol citric acid puts into 100mL, add distilled water 20mL, dissolve under magnetic stirring, form clear solution, then take 0.02mol Bismuth trinitrate, 0.036mol iron nitrate, 0.004mol aluminum nitrate successively, and add in above-mentioned citric acid solution, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned three kinds of metallic cations is 1.3:1.Second step, when constantly stirring, is 8 by ammoniacal liquor adjust ph, mixing solutions ageing 20 hours; Then in a water bath 100 DEG C by the removing of solution evaporate to dryness moisture, in an oven 170 DEG C of dryings, until form black xerogel.3rd step, fully grinds the xerogel collected, in atmosphere 600 DEG C of thermal treatment 4 hours, gets rid of organism, obtains precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 3.6al 0.4o 9ceramics sample.
Utilize the Bi that embodiment 3 prepares 2fe 3.6al 0.4o 9the XRD of multiferroic ceramics sample as shown in Figure 1, observes all diffraction peaks and the Bi of orthohormbic structure from Fig. 1 2fe 4o 9coincide, show single-phase, the diffraction peak without second-phase occurs, shows Al 3+fe can be replaced completely 3+enter into Bi 2fe 4o 9lattice in go.Fig. 2, Fig. 3 sets forth Bi 2fe 3.6al 0.4o 9magnetic hysteresis loop, ferroelectric hysteresis loop.Wherein, the curve x=0.4 that represents in Fig. 1, Fig. 2, Fig. 3 of example 2.
Embodiment 4
Utilize citric acid-nitrate sol-gel method, preparation Bi 2fe 4-xal xo 9(x=0.6) multiferroic pottery.The first step, take the beaker that 0.09mol citric acid puts into 100mL, add distilled water 20mL, dissolve under magnetic stirring, form clear solution, then take 0.02mol Bismuth trinitrate, 0.034mol iron nitrate, 0.006mol aluminum nitrate successively, and add in above-mentioned citric acid solution, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned three kinds of metallic cations is 1.5:1.Second step, when constantly stirring, is 8 by ammoniacal liquor adjust ph, mixing solutions ageing 24 hours; Then in a water bath 100 DEG C by the removing of solution evaporate to dryness moisture, in an oven 170 DEG C of dryings, until form black xerogel.3rd step, fully grinds the xerogel collected, in atmosphere 600 DEG C of thermal treatment 4 hours, gets rid of organism, obtains precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 3.4al 0.6o 9ceramics sample.
Utilize the Bi that embodiment 4 prepares 2fe 3.4al 0.6o 9the XRD of multiferroic ceramics sample as shown in Figure 1, observes all diffraction peaks and the Bi of orthohormbic structure from Fig. 1 2fe 4o 9coincide, show single-phase, the diffraction peak without second-phase occurs, shows Al 3+fe can be replaced completely 3+enter into Bi 2fe 4o 9lattice in go.Fig. 2, Fig. 3 sets forth Bi 2fe 3.4al 0.6o 9magnetic hysteresis loop, ferroelectric hysteresis loop.Wherein, the curve x=0.6 that represents in Fig. 1, Fig. 2, Fig. 3 of example 2.
Adopt Bi prepared by above method 2fe 4-xal xo 9(x=0.2,0.4,0.6) pottery possesses the single-phase room temperature multiferroic of structure, is a kind of ceramic material with broad prospect of application.To the sign of sample microtexture, adopt X-ray diffractometer (XRD) to its material phase analysis; The magnetic property of the comprehensive property test system of PPMS to sample of QuantumDesign company is adopted to measure; The ferroelectricity of the ferroelectric test macro of PrimerII to sample of RadiantTechnologies is adopted to measure.
As shown in Figure 1, give x=0,0.02,0.04,0.06 sintering temperature is the Bi sintered in 850 DEG C of air 2fe 4-xal xo 9the XRD figure spectrum of multiferroic ceramic material sample.All diffraction peaks and the Bi of orthohormbic structure is observed from Fig. 1 2fe 4o 9coincide, show single-phase, occur without second-phase diffraction peak, show Al 3+fe can be replaced completely 3+enter into Bi 2fe 4o 9lattice in go.
Fig. 2 (a)-(d) give x=0,0.02,0.04,0.06 sintering temperature is the Bi sintered in 850 DEG C of air 2fe 4-xal xo 9the room temperature hysteresis measurement result of multiferroic ceramic material sample.As can be seen from Fig. 2 (a), the room temperature magnetic hysteresis loop of x=0 sample is almost between one, performance paramagnetism.Along with Al 3+doping, sample shows weak ferromegnetism gradually, and hysteresis is more and more obvious, and this is due to Al 3+doping causes Fe 3+with Fe 3+spin Interaction is suppressed, and causes crystalline network distortion, thus causes the generation of non-colinear magnetic moment.Wherein, x=0.02, the coercive field of 0.04 and 0.06 sample is respectively 525, and 535 and 1950Oe, coercive field is along with Al 3+the increase of doping and increasing gradually.Experimental result shows, by suitable Al 3+introducing, the room-temperature ferromagnetic of sample can be improved.
Fig. 3 (a)-(d) give x=0,0.02,0.04,0.06 sintering temperature is the Bi sintered in 850 DEG C of air 2fe 4-xal xo 9multiferroic ceramic material sample is when 10Hz, and added electric field is respectively 10kV/cm, and the ferroelectric hysteresis loop measuring result of 20kV/cm, 30kV/cm, 40kV/cm, 50kV/cm, as can be seen from the figure sample all shows ferroelectricity.Under the strength of electric field of room temperature 50kV/cm, x=0, the remnant polarization of 0.02,0.04 and 0.06 sample is 0.227,0.254,0.273,0.386 μ C/cm 2, remnant polarization is along with Al 3+the increase of doping and increasing gradually.Experimental result shows, by suitable Al 3+introducing, the room temperature ferroelectricity of sample can be improved.
It should be noted last that, above embodiment is only in order to illustrate the technology implementation scheme of this material but not to limit, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.

Claims (2)

1. an Al 3+doping Bi 2fe 4-xal xo 9the preparation method of multiferroic stupalith, is characterized in that, comprises the following steps:
(1) under room temperature, first prepare citric acid solution, load weighted citric acid is put into beaker, adds distilled water, dissolve under magnetic stirring, form clear solution; Then analytically pure Bismuth trinitrate, iron nitrate, aluminum nitrate is added, and magnetic agitation, form homogeneous solution, wherein the mol ratio of citric acid and above-mentioned three kinds of metallic cations is 1:1 ~ 1.5:1, and citric acid is as complexing agent, and Bismuth trinitrate, iron nitrate, aluminum nitrate are as metallic cation source, the mol ratio of described Bismuth trinitrate, iron nitrate, aluminum nitrate is 2:(4-x): x, x=(0.2,0.4,0.6);
(2) when constantly stirring, be 7 ~ 8 by ammoniacal liquor adjust ph, mixing solutions ageing 12 ~ 24 hours; Then in a water bath 80 DEG C ~ 100 DEG C by solution evaporate to dryness removing moisture, 150 DEG C in an oven ~ 170 DEG C dryings, until form black xerogel;
(3) xerogel collected fully is ground, 500 DEG C in atmosphere ~ 600 DEG C thermal treatment 4 ~ 6 hours, get rid of organism, obtain precursor powder; Then by precursor powder grinding, compressing tablet sintering, sintering temperature is 850 DEG C, and sintering time is 2 hours, obtains Bi 2fe 4-xal xo 9ceramics sample.
2. an Al according to claim 1 3+doping Bi 2fe 4-xal xo 9the Bi that the preparation method of many iron stupalith obtains 2fe 4-xal xo 9many iron stupalith, is characterized in that, described Al 3+doping Bi 2fe 4o 9pottery has structure single-phase and room temperature many iron characteristic, wherein x=(0.2,0.4,0.6).
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CN105399339B (en) * 2015-12-18 2018-12-11 北京汽车股份有限公司 A kind of ferrous acid bismuth-based thin films and preparation method thereof containing doped chemical
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CN102838351A (en) * 2012-09-19 2012-12-26 北京工业大学 Multiferroic material and preparation method thereof
CN103058646A (en) * 2012-11-07 2013-04-24 陕西科技大学 Method for preparing Tb/Cr-codoped high-remanent-polarization BiFeO3 film by sol-gel process
CN103265281A (en) * 2013-06-19 2013-08-28 华中科技大学 Cr-doped Bi2Fe4O9 multiferroic ceramic material and preparation method thereof

Patent Citations (4)

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CN102219490A (en) * 2011-06-23 2011-10-19 常州大学 Spinel type multiferroics and synthesizing method thereof
CN102838351A (en) * 2012-09-19 2012-12-26 北京工业大学 Multiferroic material and preparation method thereof
CN103058646A (en) * 2012-11-07 2013-04-24 陕西科技大学 Method for preparing Tb/Cr-codoped high-remanent-polarization BiFeO3 film by sol-gel process
CN103265281A (en) * 2013-06-19 2013-08-28 华中科技大学 Cr-doped Bi2Fe4O9 multiferroic ceramic material and preparation method thereof

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