CN101531394A - Method for preparing barium titanate powder - Google Patents

Method for preparing barium titanate powder Download PDF

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CN101531394A
CN101531394A CN200910046840A CN200910046840A CN101531394A CN 101531394 A CN101531394 A CN 101531394A CN 200910046840 A CN200910046840 A CN 200910046840A CN 200910046840 A CN200910046840 A CN 200910046840A CN 101531394 A CN101531394 A CN 101531394A
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powder
barium titanate
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preparing barium
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CN101531394B (en
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丁西亚
沈波
翟继卫
付芳
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Tongji University
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Abstract

The invention relates to the electronic materials and devices field, in particular to a method for preparing barium titanate powder. The method for preparing flake BaTiO3 powder comprises the following steps: Bi2O3 and TiO2 are used as raw materials and KC1 or NaC1 are used as molten salts for preparing Bi4Ti3O12 powder by a molten salt method; mixed materials of BaCO3 and Bi4Ti3O12 are added with zirconia ball and ethanol or deionized water for ball milling for 20-24 hours, and after discharging and drying, the mixed materials are pre-sintered for 2-5 hours under 800-1500 DEG C to be grinded to obtain the powder containing BaTiO3; the power mixture prepared on the second step are cleaned, and nitric acid is used for cleaning the cleaned power mixture until the power mixture is acid. The powder preparing process of the invention has the characteristics of simple process, low cost and perfect performances. Mainly applied to the preparing of lead-free piezoelectric textured ceramics, the powder preparing process has important significance for promoting the research of the lead-free piezoelectric ceramics.

Description

Preparing barium titanate powder
Technical field
The invention belongs to electronic material and devices field.Be specifically related to a kind of preparing barium titanate powder.
Background technology
Piezoelectric ceramics is used widely in high-tech areas such as information, space flight as one of most important electronic material, is the requisite material of contemporary science and technology development.Along with high-speed development of science and technology, the enhancing of people's environmental consciousness, just more and more higher to the requirement of piezoceramic material.Present employed piezoceramic material is the most traditional, the most sophisticated to be the lead base stupalith, yet PbO probably accounts for 70% in these lead base materials, can cause serious harm to the environment and the mankind.So study unleaded base piezoelectric ceramic is the inexorable trend of piezoelectric ceramics development.To the requirement of leadless piezoelectric material material be preparation, use and discarded last handling process in can not work the mischief and possess good piezoelectric property again environment and human body.The leadless piezoelectric ceramics system mainly contains BaTiO now 3Based leadless piezoelectric ceramics, Bi 1/2Na 1/2TiO 3Based leadless piezoelectric ceramics, base metal niobate based leadless piezoelectric ceramic, tungsten bronze structure leadless piezoelectric ceramics, bismuth laminated leadless piezoelectric ceramic etc.The performance of leadless piezoelectric ceramics is compared with traditional lead titanate piezoelectric ceramics (abbreviating PZT as), and its piezoelectric property is on the low side, and the application on electronic devices and components can't replace PZT.Therefore, the piezoelectric property that how to improve leadless piezoelectric ceramics is the key point of problem.
The ceramic crystalline grain directional technology is a kind of effective ways that improve piezoelectric property.Template grain growth is a method commonly used in the ceramic crystalline grain directional technology, this method is to utilize topotactic reaction to make the high pottery of orientation degree, pattern based on material, at first preparation has the template crystal grain of certain orientation as kind of a crystalline substance, be distributed to then and apply a motivating force that makes its formation have certain veining structure structure in the matrix, template being aligned, finally reach the purpose of preferred orientation, thereby improve its piezoelectric property by pressure sintering, forge hot method, casting method.One of gordian technique of this method is exactly to prepare the sheet template kind crystalline substance that blade diameter length ratio is big, have orientation.Barium titanate (BaTiO 3) crystal is because of having perovskite structure, chemical property is stable, the piezo-electric modulus height, thereby the ideal that becomes kind of crystalline substance is selected.But because sheet BaTiO 3Template is difficult to preparation and the research of restriction this respect, and existing preparation technology is very complicated, and the synthetic sheet BaTiO of institute 3Powder is because of too big (50 μ m～100 μ m) the uncomfortable collaboration template kind crystalline substance of size.Therefore, study a kind of simple prepared sheet BaTiO 3Template, and its sheet size adjustable becomes problem demanding prompt solution.Control crystal growth pattern has two kinds of methods usually: directly crystalline growth and forming core growth on the previously prepared template from solution.Molten-salt growth method is a method the most frequently used in the direct growth method, and it uses fused salt as the mass transfer that reacts between oxide compound.In fused salt, because interionic has higher rate of diffusion, but therefore reaction is finished within a short period of time.
Summary of the invention
The purpose of this invention is to provide a kind of preparing barium titanate powder.
Preparing barium titanate powder principle of the present invention is:
Figure A200910046840D00041
(1)
Figure A200910046840D00042
(2)
Preparing barium titanate powder of the present invention comprises the steps:
1) with Bi 2O 3And TiO 2Be raw material, KCl or NaCl are fused salt, prepare sheet Bi by molten-salt growth method 4Ti 3O 12Powder;
2) with BaCO 3Sheet Bi with step 1 preparation 4Ti 3O 12Powder mixes and to be placed in the nylon ball grinder, adds zirconia ball and dehydrated alcohol or deionized water and carries out ball milling, carries out pre-burning with KCl or NaCl fused salt then, is incubated after being warming up to synthesis temperature then, makes after the cooling and contains BaTiO 3Powder mixture;
3) powder mixture of cleaning step 2 preparations obtains BaTiO 3Powder.
In the step 1, described Bi 4Ti 3O 12The preparation method of powder is as follows: with Bi 2O 3And TiO 2Is that according to mol ratio the 2.24:3 proportioning mixes, the KCl or the NaCl that take by weighing then with powder total mass equal mass are fused salt, 800 ℃ of insulations 1 hour and be warming up to 950 ℃ and pre-burning 2～3 hours, make sheet Bi 4Ti 3O 12Powder.
In the step 2, described BaCO3 and Bi 4Ti 3O 12Molar ratio, that is: BaCO 3: Bi 4Ti 3O 123:1, preferred, BaCO 3And Bi 4Ti 3O 12Mol ratio be 5～8:1.
In the step 2, the mass ratio of described zirconia ball and ball milling material is 1.2～1.5:1; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5～3.0:1.
In the step 2, the described ball milling time is 20～24 hours.
In the step 2, described synthesis temperature is 800 ℃～1500 ℃, is preferably 950 ℃～1080 ℃.
In the step 3, the cleaning way of described powder mixture is: use the ebullient deionized water to soak earlier 24 hours, and constantly change deionized water during the course, use ultrasonic cleaning then, clean to using AgNO 3Solution check washing back solution does not have Cl-; And then the product that will clean cleans to solution with nitric acid and is acid to remove BaCO 3And Bi 2O 3
The BaTiO that method of the present invention makes 3The particle size range of powder reaches micron order.
The present invention adopts traditional powder preparing technology, selects the Bi with excellent sheet structure for use 4Ti 3O 12Powder is the synthetic BaTiO of intermediate material 3Powder utilizes bismuth titanates to be intermediate material, with BaCO 3Different mole proportionings replace bismuth by barium and obtain highly purified sheet-like barium titanate powder within certain temperature range, can utilize this sheet-like barium titanate powder to prepare textured ceramic for template, and it has following principal feature:
(1) BaTiO of this sheet structure 3The size of powder is with sintering temperature and BaCO 3/ Bi 4Ti 3O 12Mol ratio changes, and can prepare the sheet BaTiO of distribution of sizes at 2 μ m～10 μ m 3Powder;
(2) with this sheet BaTiO 3Powder is that the prepared textured ceramic of template has excellent orientation, has improved its piezoelectric property greatly;
(3) adopt traditional powder preparing technology, technology is simple, and cost is low, and excellent performance is mainly used in the preparation of leadless piezoelectric structured pottery, and is significant to the research that promotes leadless piezoelectric ceramics.
The present invention adopts molten-salt growth method successfully to prepare the sheet BaTiO of distribution of sizes at 5 μ m～10 μ m 3Powder can be used for the kind crystalline substance of template grain growth, and not only technology is simple, cost is lower, and studies different technology and the chemical constitution rule that influences to its pattern.
Description of drawings
Fig. 1 sheet Bi 4Ti 3O 12The SEM picture of powder.
Fig. 2 embodiment 1 sheet BaTiO 3The XRD figure spectrum of powder.
Fig. 3 embodiment 2 sheet BaTiO 3The XRD figure spectrum of powder.
Fig. 4 sheet BaTiO 3The SEM picture of powder.
Fig. 5 sheet BaTiO 3The EDS collection of illustrative plates of powder.
Fig. 6 embodiment 1 sheet BaTiO 3The SEM picture of powder.
Fig. 7 embodiment 2 sheet BaTiO 3The SEM picture of powder.
Fig. 8 sheet BaTiO of preparation among the embodiment 1 3Powder is the XRD figure spectrum of the textured ceramic of template preparation.
Embodiment
Reagent source in the experiment:
Raw material and reagent producer
Bi 2O 3Shudu Electronic Powder Material Factory, Chengdu
TiO Chemical Reagent Co., Ltd., Sinopharm Group, chemical pure
KCl Chemical Reagent Co., Ltd., Sinopharm Group, analytical pure
NaCl Chemical Reagent Co., Ltd., Sinopharm Group, analytical pure
BaCO 3Chemical Reagent Co., Ltd., Sinopharm Group, analytical pure
Embodiment 1
The preparation sheet BaTiO of present embodiment 3The principle equation of powder is:
Figure A200910046840D00061
(1)
Figure A200910046840D00062
(2)
According to above chemical equation (1), prepare intermediate material sheet Bi by molten-salt growth method 4Ti 3O 12Powder.Concrete steps are as follows: take by weighing Bi 2O 3And TiO 2, Bi wherein 2O 3And TiO 2Molar ratio be 2.24:3; Selection NaCl is a fused salt, 800 ℃ of insulations 1 hour and heat up (heat-up rate be 3 ℃/min) to 950 ℃ of pre-burnings of synthesis temperature 3 hours, cool to room temperature with the furnace, can prepare sheet Bi 4Ti 3O 12Powder, Fig. 1 are sheet Bi 4Ti 3O 12The SEM picture of powder, by among Fig. 1 as can be seen, the Bi of preparation 4Ti 3O 12The particle size range of powder is 10 μ m～15 μ m.
With BaCO3 and prepared Bi 4Ti 3O 12Powder is a raw material, and selection NaCl is a fused salt, according to above chemical equation (2), can prepare sheet BaTiO 3Powder.Concrete steps are as follows: take by weighing BaCO 3And Bi 4Ti 3O 12Mol ratio be 5:1; With ethanol is ball-milling medium, and wherein the mass ratio of zirconia ball and ball milling material is 1.2:1; The mass ratio of ethanol and ball milling material is 3.0:1, and ball milling 24 hours adds NaCl in 110 ℃ of dry backs and mixes, in the corundum crucible of packing into, and the wherein quality of the NaCl of Jia Ruing and BaCO 3With prepared Bi 4Ti 3O 12The total mass of powder equates.Then above-mentioned mixed powder is warming up to 950 ℃ 800 ℃ of pre-burnings after 1 hour and is incubated 2 hours down, cool to room temperature with the furnace.Prepared powder was soaked one day earlier with the ebullient deionized water, and constantly change deionized water, use ultrasonic cleaning, until using AgNO 3Solution check washing back solution does not have Cl -(Ex-all NaCl).The product that will clean cleans repeatedly with nitric acid again, (Ex-all Bi till the solution after the washing is acidity 2O 3) promptly make sheet BaTiO 3Powder.Fig. 2 is synthetic sheet BaTiO in the present embodiment 3The XRD figure spectrum of powder.Fig. 4 and Fig. 5 are respectively sheet BaTiO 3The SEM of powder and EDS collection of illustrative plates, Fig. 6 are synthesizing flaky BaTiO in the present embodiment 3The SEM picture of powder.By among Fig. 6 as can be seen, the sheet BaTiO for preparing in the present embodiment 3The distribution of sizes scope of powder is 2 μ m～10 μ m.
Use conventional preparation method to use the above-mentioned sheet BaTiO that makes then 3Powder prepares pottery, and concrete grammar is as follows: with the sheet BaTiO for preparing in the present embodiment 3Powder and size are the BaTiO of 100nm 3The mass ratio of powder is the even and curtain coating of the mixed of 1:4, the film of curtain coating is sheared and be superimposed at the inferior static pressure of the pressure of 200MP, be 3 ℃/min heating with heat-up rate then, be warming up to 1400 ℃ of insulation 2h down, can prepare the height-oriented textured ceramic that is equipped with.Fig. 8 is with the sheet BaTiO for preparing in the present embodiment 3Powder is the XRD figure spectrum of the textured ceramic of template preparation, from then on collection of illustrative plates as can be known, its (H00) orientation degree is more than 80%.
Embodiment 2
Prepare intermediate material sheet Bi by molten-salt growth method 4Ti 3O 12Powder.Concrete steps are as follows: take by weighing Bi 2O 3And TiO 2, Bi wherein 2O 3And TiO 2Molar ratio be 2.24:3, wherein Bi 2O 3Excessive 12wt%; Selection KCl is a fused salt, 800 ℃ of insulations 1 hour and heat up (heat-up rate be 4 ℃/min) to 950 ℃ of pre-burnings of synthesis temperature 3 hours, cool to room temperature with the furnace, can prepare sheet Bi 4Ti 3O 12Powder.
With BaCO 3With prepared Bi 4Ti 3O 12Powder is a raw material, and selection KCl is a fused salt, according to above chemical equation (2), can prepare sheet BaTiO 3Powder.Concrete steps are as follows: take by weighing BaCO 3And Bi 4Ti 3O 12Mol ratio be: 7:1; With ethanol is ball-milling medium, and wherein the mass ratio of zirconia ball and ball milling material is 1.5:1; The mass ratio of ethanol and ball milling material is 1.5:1, ball milling 20 hours is in quality KCl such as 110 ℃ of dry back addings and mix, pack in the corundum crucible, be incubated 1 hour and be warming up to 1080 ℃ of following insulations of synthesis temperature 2 hours at 800 ℃, cool to room temperature with the furnace, institute's synthetic powder was soaked one day earlier with the ebullient deionized water, and constantly change deionized water, use ultrasonic cleaning, until using AgNO 3Solution check washing back solution does not have Cl -(Ex-all NaCl).The product that will clean cleans repeatedly with nitric acid again, (Ex-all Bi till the solution after the washing is acidity 2O 3).
Fig. 3 is embodiment 2 synthetic sheet BaTiO 3The XRD figure spectrum of powder, Fig. 7 is synthetic sheet BaTiO among the embodiment 2 3The SEM picture of powder.By among Fig. 7 as can be seen, the sheet BaTiO for preparing in the present embodiment 3The distribution of sizes scope of powder is 2 μ m～10 μ m.
Embodiment 3
Prepare intermediate material sheet Bi by molten-salt growth method 4Ti 3O 12Powder.Concrete steps are as follows: take by weighing Bi 2O 3And TiO 2, Bi wherein 2O 3And TiO 2Molar ratio be 2.24:3, wherein Bi 2O 3Excessive 12wt%; Selection KCl is a fused salt, 800 ℃ of insulations 1 hour and heat up (heat-up rate be 4 ℃/min) to 950 ℃ of pre-burnings of synthesis temperature 2 hours, cool to room temperature with the furnace, can prepare sheet Bi 4Ti 3O 12Powder.
With BaCO 3With prepared Bi 4Ti 3O 12Powder is a raw material, and selection KCl is a fused salt, according to above chemical equation (2), can prepare sheet BaTiO 3Powder.Concrete steps are as follows: take by weighing BaCO 3And Bi 4Ti 3O 12Mol ratio be 8:1; With ethanol is ball-milling medium, and wherein the mass ratio of zirconia ball and ball milling material is 1.4:1; The mass ratio of ethanol and ball milling material is 2.0:1, ball milling 20 hours is in quality KCl such as 110 ℃ of dry back addings and mix, pack in the corundum crucible, be incubated 1 hour and be warming up to 1500 ℃ of following pre-burnings of synthesis temperature 2 hours at 800 ℃, grind then after 4 hours and cool to room temperature with the furnace, institute's synthetic powder was soaked one day earlier with the ebullient deionized water, and constantly change deionized water, use ultrasonic cleaning, until using AgNO 3Solution check washing back solution does not have Cl -(Ex-all NaCl).The product that will clean cleans repeatedly with nitric acid again, (Ex-all Bi till the solution after the washing is acidity 2O 3).

Claims (7)

1. a preparing barium titanate powder comprises the steps:
1) with Bi 2O 3And TiO 2Be raw material, KCl or NaCl are fused salt, prepare sheet Bi by molten-salt growth method 4Ti 3O 12Powder;
2) with BaCO 3Sheet Bi with step 1 preparation 4Ti 3O 12Powder mixes and to be placed in the nylon ball grinder, adds zirconia ball and dehydrated alcohol or deionized water and carries out ball milling, carries out pre-burning with KCl or NaCl fused salt then, is incubated after being warming up to synthesis temperature then, makes after the cooling and contains BaTiO 3Powder mixture;
3) cleaning step 2 preparation contains BaTiO 3Powder mixture obtain BaTiO 3Powder.
2, preparing barium titanate powder as claimed in claim 1 is characterized in that, sheet Bi in the described step 1) 4Ti 3O 12The preparation method of powder is: with Bi 2O 3And TiO 2Is that according to mol ratio the 2.24:3 proportioning mixes, the KCl or the NaCl that take by weighing then with powder total mass equal mass are fused salt, 800 ℃ of insulations 1 hour and be warming up to 950 ℃ of pre-burnings 2～3 hours, make sheet Bi 4Ti 3O 12Powder.
3, preparing barium titanate powder as claimed in claim 1 is characterized in that, described step 2) middle BaCO 3With Bi 4Ti 3O 12The molar ratio scope be 5:1～8:1.
4, preparing barium titanate powder as claimed in claim 1 is characterized in that, described step 2) in synthesis temperature be 950 ℃～1080 ℃.
5, preparing barium titanate powder as claimed in claim 1 is characterized in that, described step 2) in the mass ratio of zirconia ball and ball milling material be 1.2～1.5:1.
6, preparing barium titanate powder as claimed in claim 1 is characterized in that, described step 2) in the mass ratio of dehydrated alcohol or deionized water and ball milling material be 1.5～3.0:1.
7, preparing barium titanate powder as claimed in claim 1, it is characterized in that the cleaning way of the powder mixture in the described step 3) is: use the ebullient deionized water to soak earlier 24 hours, and constantly change deionized water during the course, use ultrasonic cleaning then, clean to using AgNO 3Solution check washing back solution does not have Cl -And then the product that will clean cleans to solution with nitric acid and is acid.
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Cited By (10)

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CN102276255A (en) * 2011-06-02 2011-12-14 西北工业大学 Preparation method for sheet-like barium titanate microcrystalline powder
CN101805178B (en) * 2010-01-22 2012-06-13 华中科技大学 High-energy ball milling preparation method of barium titanate-based semiconductor ceramics
CN103030391A (en) * 2012-12-10 2013-04-10 广西新未来信息产业股份有限公司 Bismuth titanate modified barium titanate base positive temperature coefficient resistance material and fabrication method thereof
CN104261483A (en) * 2012-11-29 2015-01-07 江苏理工学院 Method for preparing ferrate nanosheet
CN109205662A (en) * 2018-11-21 2019-01-15 北京工业大学 Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron
CN109608196A (en) * 2019-01-04 2019-04-12 同济大学 A method of synthesizing of uniform size, good dispersion flaky sodium niobate powder
CN113830829A (en) * 2021-09-30 2021-12-24 西安交通大学 Flaky bismuth titanate strontium barium template crystal grain and preparation method thereof
CN114132967A (en) * 2021-12-03 2022-03-04 西安建筑科技大学 Preparation method of calcium manganate thermoelectric microcrystal powder with flaky perovskite structure
CN115073166A (en) * 2022-06-16 2022-09-20 西安交通大学 High-temperature piezoelectric textured ceramic, template and preparation method thereof
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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101805178B (en) * 2010-01-22 2012-06-13 华中科技大学 High-energy ball milling preparation method of barium titanate-based semiconductor ceramics
CN102276255A (en) * 2011-06-02 2011-12-14 西北工业大学 Preparation method for sheet-like barium titanate microcrystalline powder
CN104261483A (en) * 2012-11-29 2015-01-07 江苏理工学院 Method for preparing ferrate nanosheet
CN104261483B (en) * 2012-11-29 2016-02-03 江苏理工学院 A kind of method preparing wustite nano flake
CN103030391A (en) * 2012-12-10 2013-04-10 广西新未来信息产业股份有限公司 Bismuth titanate modified barium titanate base positive temperature coefficient resistance material and fabrication method thereof
CN109205662A (en) * 2018-11-21 2019-01-15 北京工业大学 Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron
CN109608196A (en) * 2019-01-04 2019-04-12 同济大学 A method of synthesizing of uniform size, good dispersion flaky sodium niobate powder
CN109608196B (en) * 2019-01-04 2021-10-08 同济大学 Method for synthesizing flaky sodium niobate powder with uniform size and good dispersibility
CN113830829A (en) * 2021-09-30 2021-12-24 西安交通大学 Flaky bismuth titanate strontium barium template crystal grain and preparation method thereof
CN114132967A (en) * 2021-12-03 2022-03-04 西安建筑科技大学 Preparation method of calcium manganate thermoelectric microcrystal powder with flaky perovskite structure
CN114132967B (en) * 2021-12-03 2024-01-16 西安建筑科技大学 Preparation method of flaky perovskite structure calcium manganate thermoelectric microcrystalline powder
CN115073166A (en) * 2022-06-16 2022-09-20 西安交通大学 High-temperature piezoelectric textured ceramic, template and preparation method thereof
CN115073166B (en) * 2022-06-16 2023-03-28 西安交通大学 High-temperature piezoelectric textured ceramic, template and preparation method thereof
CN115959704A (en) * 2022-12-08 2023-04-14 北京科技大学 Preparation method of flaky barium titanate template seed crystal
CN115959704B (en) * 2022-12-08 2024-04-02 北京科技大学 Preparation method of flaky barium titanate template seed crystal

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