CN103193476B - A Wet Chemical Method for Preparing Pure Phase BiFeO3 Ceramics - Google Patents
A Wet Chemical Method for Preparing Pure Phase BiFeO3 Ceramics Download PDFInfo
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- CN103193476B CN103193476B CN201310160017.9A CN201310160017A CN103193476B CN 103193476 B CN103193476 B CN 103193476B CN 201310160017 A CN201310160017 A CN 201310160017A CN 103193476 B CN103193476 B CN 103193476B
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 239000000126 substance Substances 0.000 title claims abstract description 15
- 229910002902 BiFeO3 Inorganic materials 0.000 title abstract 2
- 239000000843 powder Substances 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims description 16
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 14
- 229940095064 tartrate Drugs 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 abstract 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 abstract 1
- 239000007769 metal material Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 235000002906 tartaric acid Nutrition 0.000 abstract 1
- 239000011975 tartaric acid Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000005291 magnetic effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000005621 ferroelectricity Effects 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007775 ferroic material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- Magnetic Ceramics (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明提供制备纯相BiFeO3陶瓷的湿化学方法，涉及无机非金属材料领域。该方法为：将Fe(NO3)3·9H2O和Bi(NO3)3·5H2O溶于水，加入酒石酸，然后在90-150℃持续搅拌，直到溶液为粘稠状，停止搅拌，烘干，在380-420℃预烧3-5h，研磨后得到前驱物粉末；将前驱物粉末在500-600℃预烧2-4h得到BiFeO3粉末；将BiFeO3粉末研磨、压片后得到BiFeO3陶瓷胚体；将BiFeO3陶瓷胚体在700-800℃密封烧结1-2h，得到纯相BiFeO3陶瓷。本发明工艺简单，得到的纯相BiFeO3陶瓷致密，颗粒的大小可以通过烧结温度进行调控。
The invention provides a wet chemical method for preparing pure-phase BiFeO3 ceramics, and relates to the field of inorganic non-metallic materials. The method is: dissolve Fe(NO 3 ) 3 ·9H 2 O and Bi(NO 3 ) 3 ·5H 2 O in water, add tartaric acid, and then keep stirring at 90-150°C until the solution is viscous and stop Stir, dry, pre-calcine at 380-420°C for 3-5h, grind to obtain precursor powder; pre-sinter the precursor powder at 500-600°C for 2-4h to obtain BiFeO 3 powder; grind and press BiFeO 3 powder Finally, a BiFeO 3 ceramic green body is obtained; the BiFeO 3 ceramic green body is sealed and sintered at 700-800° C. for 1-2 hours to obtain a pure-phase BiFeO 3 ceramic. The process of the invention is simple, and the obtained pure-phase BiFeO 3 ceramics are dense, and the particle size can be regulated through the sintering temperature.
Description
Technical field
The present invention relates to field of inorganic nonmetallic material, be specifically related to one and prepare pure phase BiFeO
3the wet chemical method of pottery.
Background technology
Multi-ferroic material, make it can be widely used in the high-tech sectors such as transverter, sensor, multiple-state storage because there is ferroelectricity, ferromegnetism and ferroelasticity (having wherein two kinds of performances at least) and consequent coupling effect simultaneously, cause scientists broad interest, and become the study hotspot in Materials Science and Engineering field.
BiFeO
3that one has the triangle distorted perovskite structure typical multi-ferroic material of (belonging to R3C space group).Under room temperature, have simultaneously ferroelectric order (
t c=1103 K) and G type antiferromagnetic order (
t n=643 K), be under minority room temperature, to there is one of ferroelectricity and ferromagnetic monophase materials simultaneously.Although find very early BiFeO
3in the ferroelectricity and the ferromegnetism that coexist, but due to large leakage conductance makes its ferroelectricity cannot Measurement accuracy, simultaneously room temperature magnetic a little less than, these features have limited its application greatly.
Due to BiFeO
3stable warm area narrower, adopt traditional solid reaction process to be difficult to avoid other dephasign as Bi
2fe
4o
9, Bi
2.5feO
40generation.Meanwhile, the synthetic BiFeO of solid phase method
3temperature higher, Bi is volatile, can cause the skew of stoichiometric ratio.Thereby, pure phase BiFeO
3the preparation of pottery is very difficult.In early days, the people such as M.Mahesh (M.Mahesh Kumar, et al., Applied Physics Letters 76,2764 (2004)) first adopt traditional solid reaction process to prepare the BiFeO that contains dephasign
3pottery, then cleans dephasign wherein with rare nitric acid, thereby obtains single-phase BiFeO
3pottery.(Chinese patent, the publication number CN 1686932A) BiFeO to sintering such as the Zhang Shantao of Nanjing University
3pottery carries out quick cooling process, adopts quench method to prepare single-phase BiFeO
3pottery.Aspect the preparation of ceramic powder, conventional solid-state method need obtain powder through the ball milling of long period, has increased the input of processing step and equipment, and cost is higher.
Wet chemical methods has that low, the each component of temperature of reaction is mixed on molecular level, product good uniformity, purity are high, easy control of reaction system and the advantage such as energy-efficient, is widely used in the preparation of high-quality electronic ceramics powder.Prepare BiFeO with wet chemistry method
3the correlative study report of pottery is few.Cao Chuanbao etc. (Chinese patent, publication number CN 102225865A) first obtain BiFeO by sol-gel method
3xerogel, then carries out twice preheating, after last compressing tablet, at 450-550 DEG C of sintering, obtains the single-phase BiFeO that particle diameter is less than 62nm
3pottery, has saturated magnetic hysteresis loop.But because the ceramic particle of preparation is less, hole is many, fine and close not, the leakage current of system is larger.
Summary of the invention
The object of the present invention is to provide one to prepare pure phase BiFeO
3the wet chemical method of pottery, technique is simple, the pure phase BiFeO obtaining
3ceramic dense, the size of particle can regulate and control by sintering temperature.
In order to realize above-mentioned aspect object, the present invention adopts following technical scheme:
One is prepared pure phase BiFeO
3the wet chemical method of pottery, comprises the following steps:
(1) by Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2o is water-soluble, obtains mixing solutions;
(2) tartrate is dissolved in the described mixing solutions of step (1), then continues to stir at 90-150 DEG C, until solution is thick, stop stirring, dry, at 380-420 DEG C of pre-burning 3-5h, after grinding, obtain precursor powder;
(3) described step (2) precursor powder is obtained to BiFeO at 500-600 DEG C of pre-burning 2-4h
3powder; By described BiFeO
3after powder grinding, compressing tablet, obtain BiFeO
3pottery idiosome; By described BiFeO
3pottery idiosome, at 700-800 DEG C of sealed sintering 1-2h, obtains pure phase BiFeO
3pottery.
Fe (NO in step (1)
3)
39H
2o and Bi (NO
3)
35H
2the mol ratio of O is 1:1.
Fe in step (2) unresolvable tartaric acid and the described mixing solutions of step (1)
3+and Bi
3+the mol ratio of summation is 1:1.
Pressure when the middle compressing tablet of step (3) is 10 ~ 12 Mpa.
In step (3) by described BiFeO
3pottery idiosome is embedded in BiFeO
3in powder, then just carry out sealed sintering.
After sealed sintering, grind off described pure phase BiFeO
3the dirt settling of ceramic surface; Described surface attachments is by BiFeO
3powder forms in sealed sintering process.
Beneficial effect: the present invention prepares pure phase BiFeO
3the wet chemical method of pottery, technique is simple, the pure phase BiFeO obtaining
3ceramic dense, the size of particle can regulate and control by sintering temperature.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram (XRD) of sample 1.
Fig. 2 is the field emission scanning electron microscope figure (SEM) of sample 1.
Fig. 3 is the field emission scanning electron microscope figure (SEM) of sample 2
Fig. 4 is the field emission scanning electron microscope figure (SEM) of sample 3.
Embodiment
Embodiment 1
Preparation pure phase BiFeO
3the wet chemical method of pottery, comprises the following steps:
(1) use analytically pure Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2o, as raw material, mixes according to mol ratio 1:1, adds deionized water, by magnetic agitation, raw material is dissolved completely, becomes uniform mixing solutions;
(2) take analytically pure tartrate, Fe in the described mixing solutions of tartrate and step (1)
3+with Bi
3+the mol ratio of ion summation is 1:1.Tartrate is added in the described mixing solutions of step (1), stir and make tartrate dissolve completely and mix; Then continue to stir at 100 DEG C, until that solution becomes is thick, stop stirring, at 100 DEG C, dry, then reaction vessel is transferred in retort furnace, at 400 DEG C of pre-burning 4h, remove organism, then, through grinding, obtain precursor powder;
(3) by obtain precursor powder transfer to alumina crucible, at 500 DEG C of pre-burning 2h, obtain BiFeO
3powder.By gained BiFeO
3powder obtains BiFeO at the pressure lower sheeting of 10 Mpa after grinding
3pottery idiosome
.in alumina crucible, put into BiFeO
3powder, by BiFeO
3pottery idiosome is imbedded BiFeO
3in powder, cover lid is sealed sintering 1h in the time of 700 DEG C, finally grinds off the dirt settling of ceramic surface, obtains sample 1.Surface attachments is by BiFeO
3powder forms in sealed sintering process, and they can be bonded in ceramic surface, is easy to grind off.
In sealed sintering process, by BiFeO
3pottery idiosome is imbedded BiFeO
3powder, is because Bi easily volatilizees, in sealed sintering process, and BiFeO
3bi in powder can first volatilize, and forms the atmosphere of Bi element relative saturation in closed environment, thereby stops BiFeO
3bi volatilization in pottery idiosome, reduces ceramic defect.
The X-ray diffractogram (XRD) of sample 1 as shown in Figure 1, the diffraction peak that can observe and the BiFeO of standard
3, there is not other impurity peaks in (JCPDS No. 21-0169) unanimously.The BiFeO that this illustrative material 1 is pure phase
3pottery.Fig. 2 is the field emission scanning electron microscope figure (SEM) of sample 1.As can be seen from the figure, ceramic dense, tight, greatly about 2-3 μ m, there are some little crystal grain in its particle size.
Embodiment 2
Preparation pure phase BiFeO
3the wet chemical method of pottery, comprises the following steps:
(1) use analytically pure Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2o, as raw material, after mixing, adds deionized water according to mol ratio 1:1, by magnetic agitation, raw material is dissolved completely, becomes uniform mixing solutions;
(2) take analytically pure tartrate, Fe in the described mixing solutions of tartrate and step (1)
3+with Bi
3+ion summation mol ratio be 1:1.Tartrate is added in the described mixing solutions of step (1), stir and make tartrate dissolve completely and mix; Then continue to stir at 120 DEG C, until that solution becomes is thick, stop stirring, dry 120 DEG C of conditions, then reaction vessel is transferred in retort furnace, at 380 DEG C of pre-burning 3h, remove organism, then grinding, obtains precursor powder;
(3) by obtain precursor powder transfer to alumina crucible, at 600 DEG C of pre-burning 2h, obtain BiFeO
3powder.By BiFeO
3powder obtains BiFeO at the pressure lower sheeting of 12 Mpa after grinding
3pottery idiosome
.in alumina crucible, put into BiFeO
3powder, at BiFeO
3in powder, imbed BiFeO
3pottery idiosome, cover lid is sealed sintering 1.5h in the time of 750 DEG C, finally grinds off the dirt settling of ceramic surface, obtains sample 2.Surface attachments is by BiFeO
3powder forms in sealed sintering process, and they can be bonded in ceramic surface, is easy to grind off.
Sample 2 is carried out to X-ray diffraction, find out the BiFeO of diffraction peak and standard
3, there is not other impurity peaks in (JCPDS No. 21-0169) unanimously.The BiFeO that this interpret sample 2 is pure phase
3pottery.
Fig. 3 is the field emission scanning electron microscope figure (SEM) of sample 2.As can be seen from the figure, ceramic dense, tight, its particle size is greatly about 2 ~ 4 μ m.
Embodiment 3
Preparation pure phase BiFeO
3the wet chemical method of pottery, comprises the following steps:
(1) use analytically pure Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2o, as raw material, after being 1:1 weighing, adds deionized water according to mol ratio, by magnetic agitation, raw material is dissolved completely, becomes uniform mixing solutions;
(2) take analytically pure tartrate, Fe in the described mixing solutions of tartrate and step (1)
3+with Bi
3+ion summation mol ratio be 1:1.Tartrate is added in the described mixing solutions of step (1), stir and make tartrate dissolve completely and mix; Then continue to stir at 150 DEG C, until that solution becomes is thick, stop stirring, under 150 DEG C of conditions, dry, then reaction vessel is transferred in retort furnace, at 420 DEG C of pre-burning 4.5h, remove organism, then, through grinding, obtain precursor powder;
(3) by obtain precursor powder transfer to alumina crucible, at 550 DEG C of pre-burning 2.5h, obtain BiFeO
3powder.By BiFeO
3powder obtains BiFeO at the pressure lower sheeting of 11 Mpa after grinding
3pottery idiosome.In alumina crucible, put into BiFeO
3powder, at BiFeO
3in powder, imbed BiFeO
3pottery idiosome, cover lid is sealed sintering 1h in the time of 800 DEG C, finally grinds off the dirt settling of ceramic surface, obtains sample 3.Surface attachments is by BiFeO
3powder forms in sealed sintering process, and they can be bonded in ceramic surface, is easy to grind off.
Sample 3 is carried out to X-ray diffraction, find out the BiFeO of diffraction peak and standard
3, there is not other impurity peaks in (JCPDS No. 21-0169) unanimously.The BiFeO that this illustrative material 3 is pure phase
3pottery.
Fig. 4 is the field emission scanning electron microscope figure (SEM) of sample 3.As can be seen from the figure, ceramic dense, tight, its particle size is greatly about 4 ~ 5 μ m.
Claims (4)
1. prepare pure phase BiFeO for one kind
3the wet chemical method of pottery, is characterized in that comprising the following steps:
(1) by Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2o is water-soluble, obtains mixing solutions; Wherein Fe (NO
3)
39H
2o and Bi (NO
3)
35H
2the mol ratio of O is 1:1;
(2) tartrate is dissolved in the described mixing solutions of step (1), then continues to stir at 90-150 DEG C, until solution is thick, stop stirring, dry, at 380-420 DEG C of pre-burning 3-5h, after grinding, obtain precursor powder; Fe in the described mixing solutions of its unresolvable tartaric acid and step (1)
3+and Bi
3+the mol ratio of summation is 1:1;
(3) described step (2) precursor powder is obtained to BiFeO at 500-600 DEG C of pre-burning 2-4h
3powder; By described BiFeO
3after powder grinding, compressing tablet, obtain BiFeO
3pottery idiosome; By described BiFeO
3pottery idiosome, at 700-800 DEG C of sealed sintering 1-2h, obtains pure phase BiFeO
3pottery.
2. prepare according to claim 1 pure phase BiFeO
3the wet chemical method of pottery, is characterized in that: pressure when the middle compressing tablet of step (3) is 10 ~ 12 Mpa.
3. prepare according to claim 1 pure phase BiFeO
3pottery wet chemical method, it is characterized in that: in step (3) by described BiFeO
3pottery idiosome is embedded in BiFeO
3in powder, then just carry out sealed sintering.
4. preparation pure phase BiFeO according to claim 3
3the wet chemical method of pottery, is characterized in that: after sealed sintering, grind off described pure phase BiFeO
3the dirt settling of ceramic surface; Described surface attachments is by BiFeO
3powder forms in sealed sintering process.
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|---|---|---|---|
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| CN103193476B true CN103193476B (en) | 2014-11-26 |
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| CN104659080A (en) * | 2015-02-04 | 2015-05-27 | 天津师范大学 | Multiferroic nanoparticles with threshold switching effect and preparation method thereof |
| CN105203598B (en) * | 2015-10-08 | 2018-04-06 | 江苏科技大学 | A kind of bismuth ferrite gas sensitive of quick response and its application |
| CN116283339A (en) * | 2023-04-11 | 2023-06-23 | 昆明理工大学 | Preparation method of pure-phase bismuth ferrite ceramic |
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| CN102173764B (en) * | 2011-01-11 | 2013-02-27 | 桂林理工大学 | A kind of bismuth ferrite-based multiferroic material and preparation method thereof |
| CN102583566A (en) * | 2011-01-20 | 2012-07-18 | 西北工业大学 | Preparation method for bismuth ferrate nano fibers |
| CN102583569B (en) * | 2012-02-16 | 2014-04-16 | 陕西科技大学 | Method for preparing bismuth ferrite film with dielectric property by adopting liquid-phase self-assembly technology |
| CN102583571A (en) * | 2012-02-29 | 2012-07-18 | 南京信息工程大学 | A kind of wet chemical preparation method of Bi2Fe4O9 nanopowder |
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