CN109205662A - Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron - Google Patents

Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron Download PDF

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CN109205662A
CN109205662A CN201811394020.6A CN201811394020A CN109205662A CN 109205662 A CN109205662 A CN 109205662A CN 201811394020 A CN201811394020 A CN 201811394020A CN 109205662 A CN109205662 A CN 109205662A
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micron
brilliant
sheet
fused salt
microns
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CN109205662B (en
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侯育冬
付靖
付雨童
郑木鹏
朱满康
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Beijing University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/006—Alkaline earth titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like

Abstract

Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron, belongs to electron ceramic material technical field.By two step molten-salt growth methods, with first step fused salt process, BaCO3And anatase TiO2As raw material, NaCl and KCl (NaCl:KCl=1:1) eutectic salts are as medium, in the Ba that 950~1050 DEG C obtain6Ti17O40Piece is as template, in second step fused salt process, synthesizes the sheet BaTiO of pure phase3The brilliant material of micron.Production method simple process of the present invention, low energy consumption, sheet BaTiO3Micron is brilliant to have big diameter thickness ratio, pattern more uniform.Sheet BaTiO can largely be prepared by providing one kind3The brilliant new way of micron.

Description

Two step molten-salt growth methods prepare sheet BaTiO3The brilliant method of micron
Technical field
The invention belongs to electronic information material fields, and in particular to a kind of sheet BaTiO3The brilliant preparation method of micron.
Background technique
In recent years, with the development of electronic information technology, the ferroelectric material of superior performance has become field of electronic materials Research emphasis.Monocrystal material has excellent performance compared to polycrystalline ceramics, but preparation process is complicated, at high cost, and has The textured ceramic of higher crystal orientation is shown equally better than polycrystalline No yield point ceramics better performance, but needs to obtain size equal Even consistent flaky material is as seed crystal cooperation casting technique preparation.BaTiO3It is a kind of electronic ceramics material that development is more mature The pattern of material, preparation method and corresponding product is also varied, and it can be used as seed crystal material preparation accordingly Textured ceramic, but the BaTiO of sheet-like morphology3Preparation method explored there is still a need for further.
BaTiO3It is at room temperature perovskite structure, by [TiO6] octahedron top connection altogether, Ba2+Gap is occupied, particle exists It more than certain size is difficult to generate sheet-like morphology under general condition due to the symmetry of structure for tetragonal phase for (> 30 nanometers), and Pass through a kind of one-dimensional material Ba with similar base unit6Ti17O40As template, can be made by certain condition basic single Member reassembles into required structure.In view of the importance in textured ceramic preparation of flaky material, a kind of simple and reliable method is found Prepare the BaTiO of sheet3Material is also significantly.
Molte-salt synthesis (Molten salt synthesis, MSS) be it is a kind of using fuse salt make reaction promoter preparation multiple groups Divide the straightforward procedure of single-phase powder.The single-phase powder of a large amount of multicomponents such as binary and ternary are prepared for by the method in past people Oxide ferrite and sulfide etc., if these compounds are usually required using conventional solid reaction process preparation more than 1100 DEG C, and due to the stronger mass transfer diffusion rate of fused-salt medium, it can be made at relatively low temperature by fuse salt rule, And appearance and size is uniform.Up to the present, sheet BaTiO is prepared using simple two steps molte-salt synthesis3Micron is brilliant to be also rarely reported.
Summary of the invention
It is an object of the present invention to provide can largely generate with sheet BaTiO3The brilliant preparation method of micron.Pass through two Walk molten-salt growth method, the Ba obtained with first step molten-salt growth method6Ti17O40Piece synthesizes the sheet BaTiO of pure phase as template3The brilliant material of micron Material.
The present invention is used with Ba6Ti17O40Piece is the fused salt topology synthetic method of template, it is characterized in that passing through fused salt, forerunner The selection of body and the control of process conditions prepare sheet BaTiO3Micron is brilliant, specifically uses method comprising the following steps:
Raw material: barium source raw material is using the pure BaCO of analysis3, titanium source raw material use Anatase TiO2；Fused salt auxiliary agent NaCl/ KCl。
(1) the barium source raw material, titanium source raw material and fused salt auxiliary agent of metering are pressed BaCO by first step fused salt process3: TiO2: The mixing of NaCl:KCl=6.6:17:170:170 molar ratio；
(2) obtained mixture hand-ground is obtained into uniformed powder.
(3) obtained powder is placed in crucible, 950~1050 DEG C of calcining 5h in Muffle furnace is placed in, after obtaining calcining Product A and fused salt mixture；
(4) by the mixture furnace cooling of step (3) products therefrom and fused salt, drying is washed, Ba is obtained6Ti17O40Monocrystalline Piece；
With deionized water dissolving, centrifuge washing for several times, and uses AgNO3Solution is detected to cannot find Cl?Until ion.It adopts With oven drying, drying time is 6~12h.
By above-mentioned steps, obtained product A is white Ba6Ti17O40Single-chip, diameter are about 5 microns to 15 microns, Thickness is about 0.4 to 0.7 micron.
(5) second step fused salt process, by Ba obtained by step (4)6Ti17O40As titanium source and part barium source and barium source raw material, Fused salt auxiliary agent presses Ba6Ti17O40: BaCO3: the molar ratio 1:11:120:120 mixing of NaCl:KCl；
(6) obtained mixture hand-ground is obtained to uniformed powder；
(7) obtained powder is placed in crucible, is placed in Muffle furnace 750~1050 DEG C (preferably 1000-1050 DEG C) 5h is calcined, the mixture of calcined product B and fused salt are obtained；
(8) washing after calcined mixture furnace cooling is dried to obtain product B i.e. sheet BaTiO3Micron is brilliant；
By above-mentioned steps, the sheet BaTiO is obtained3Micron is brilliant.Resulting sheet BaTiO3Product be it is faint yellow, Its diameter is about 6 microns to 19 microns, and thickness is about 0.9 to 1.3 micron.
The present invention has the advantages that following main compared with prior art:
First, process flow is simple, it is reproducible, and raw materials used is general industry raw material, it is cheap, it can be a large amount of Preparation.
Second, not using toxic organo-metallic compound in preparation, toxic addition product is not generated, combinational environment is wanted It asks.
Third, having a wide range of application.As a kind of ferroelectric material for having wide application, sheet BaTiO3Micron crystalline substance can answer extensively For application fields such as nano-device, textured ceramic, composite materials.
Detailed description of the invention (and the comparative example 1 and 2 in attached 1 is changed to 2 embodiment 3 of embodiment)
Fig. 1 product A (sheet Ba6Ti17O40), embodiment 1-2 (sheet BaTiO3Micron is brilliant) XRD diagram.
Fig. 2 product A (sheet Ba6Ti17O40), (the sheet BaTiO of embodiment 13Micron is brilliant) morphology characterization figure.
Wherein a is product A (sheet Ba6Ti17O40) SEM figure；C is its TEM electron microscope；
Wherein b is (the sheet BaTiO of embodiment 13Micron is brilliant) SEM figure；D is its TEM electron microscope.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not It is limited only to the following examples.
Embodiment 1:
1. raw material: analyzing pure BaCO3, Anatase TiO2；Fused salt auxiliary agent NaCl/KCl.
2. preparing sheet BaTiO in accordance with the following steps3Micron is brilliant
1) is by above-mentioned raw materials and fused salt auxiliary agent, BaCO3: TiO2: NaCl:KCl 6.6:17:170:170 in molar ratio Ratio mixing；
2) is by the mixture hand-ground 30min of step 1)；
3) mixture that obtains step 2) is placed in corundum crucible, 1000 DEG C of heat preservation 5h in Muffle furnace；
4) after the mixture furnace cooling of step 3) product A and fused salt, will be washed with deionized repeatedly, be collected by centrifugation, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl-Ion, dry 6~12h, obtains white in 100 DEG C of baking ovens Ba6Ti17O40Sheet output；
Ba6Ti17O40The XRD diagram of sheet output is shown in that Fig. 1, SEM figure are shown in that Fig. 2 (a), TEM figure are shown in Fig. 2 (c).
Ba in Fig. 16Ti17O40The position of each diffraction maximum of piece and relative intensity with PDF card (PDF#71-2110) main peak phase It coincide, the disappearance of individual diffraction maximums is derived from sheet Ba6Ti17O40Preferred orientation, show product be monoclinic phase Ba6Ti17O40, XRD There is no other diffraction maximums in map, illustrates to have obtained the Ba of single object phase6Ti17O40。
From Fig. 2 (a) it can be seen that synthetic product pattern be sheet, diameter be 5 microns to 15 microns, thickness be about 0.4 to 0.6 micron.
Fig. 2 (c) has further demonstrated that prepared Ba6Ti17O40Piece is monocrystal, and crystallinity is good.
The product that analysis test shows is pure phase Ba6Ti17O40Single-chip.
5) is by following raw materials and fused salt auxiliary agent B a6Ti17O40: BaCO3: NaCl:KCl 1:11:120:120 in molar ratio Ratio mixing；
6) is by the mixture hand-ground 30min of step 5)；
7) mixture that obtains step 6) is placed in corundum crucible, 1000 DEG C of heat preservation 5h in Muffle furnace；
8) is washed with deionized repeatedly, is collected by centrifugation by step 7) product B and molten salt mixture after furnace cooling, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl?Ion, dry 6~12h, obtains faint yellow in 100 DEG C of baking ovens Sheet BaTiO3The brilliant product of micron.
The sheet BaTiO of embodiment 13The brilliant XRD diagram of micron is shown in Fig. 1, the position of its each diffraction maximum and relative intensity in Fig. 1 It matches with PDF card (PDF#76-0744), shows that product is tetragonal phase BaTiO3, there is no other diffraction in XRD spectrum Peak illustrates to have obtained the BaTiO of single object phase3。
From Fig. 2 (b) it can be seen that synthetic product pattern be sheet, diameter be 6 microns to 19 microns, thickness be about 0.9 to 1.3 micron.
Fig. 2 (d) has further demonstrated that prepared sheet BaTiO3For monocrystal, crystal structure and PDF card (PDF# 76-0744) match.
The product that analysis test shows is pure phase sheet BaTiO3Micron is brilliant.
This embodiment example illustrates sheet BaTiO3The brilliant preparation method of micron, can be big using technical solution of the present invention Batch preparation sheet BaTiO3Micron is brilliant, the preparation so as to cooperate casting technology, for textured ceramic.
Embodiment 2:
1. raw material: analyzing pure BaCO3, Anatase TiO2；Fused salt auxiliary agent NaCl/KCl.
2. preparing sheet BaTiO in accordance with the following steps3Micron is brilliant
1) is by above-mentioned raw materials and fused salt auxiliary agent, BaCO3: TiO2: NaCl:KCl 6.6:17:170:170 in molar ratio Ratio mixing；
2) is by the mixture hand-ground 30min of step 1)；
3) mixture that obtains step 2) is placed in corundum crucible, 1000 DEG C of heat preservation 5h in Muffle furnace.
4) after the mixture furnace cooling of step 3) product A and fused salt, will be washed with deionized repeatedly, be collected by centrifugation, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl-Ion, dry 6~12h, obtains white in 100 DEG C of baking ovens Ba6Ti17O40Sheet output.
5) is by following raw materials and fused salt auxiliary agent B a6Ti17O40: BaCO3: NaCl:KCl 1:11:120:120 in molar ratio Ratio mixing；
6) is by the mixture hand-ground 30min of step 5)；
7) mixture that obtains step 6) is placed in corundum crucible, in Muffle furnace 850~950 DEG C it is (specifically more It is few, or you in the range of float) heat preservation 5h；
8) is washed with deionized repeatedly, is collected by centrifugation by step 7) product B and molten salt mixture after furnace cooling, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl?Ion, dry 6~12h, obtains faint yellow in 100 DEG C of baking ovens Sheet BaTiO3The brilliant product of micron.
The BaTiO of comparative example 13The XRD diagram of product is shown in Fig. 1, BaTiO in Fig. 13The position of each diffraction maximum and relative intensity are equal It matches with PDF card (PDF#76-0744), shows that product is tetragonal phase BaTiO3, but there are a small amount of raw materials to spread out in XRD spectrum Penetrate peak.
Embodiment 3:
1. raw material: analyzing pure BaCO3, Anatase TiO2；Fused salt auxiliary agent NaCl/KCl.
2. preparing sheet BaTiO in accordance with the following steps3Micron is brilliant
1) is by above-mentioned raw materials and fused salt auxiliary agent, BaCO3: TiO2: NaCl:KCl 6.6:17:170:170 in molar ratio Ratio mixing；
2) is by the mixture hand-ground 30min of step 1)；
3) mixture that obtains step 2) is placed in corundum crucible, 1000 DEG C of heat preservation 5h in Muffle furnace.
4) after the mixture furnace cooling of step 3) product A and fused salt, will be washed with deionized repeatedly, be collected by centrifugation, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl-Ion, dry 6~12h, obtains white in 100 DEG C of baking ovens Ba6Ti17O40Sheet output.
5) is by following raw materials and fused salt auxiliary agent B a6Ti17O40: BaCO3: NaCl:KCl 1:11:120:120 in molar ratio Ratio mixing；
6) is by the mixture hand-ground 30min of step 5)；
7) mixture that obtains step 6) is placed in corundum crucible, in Muffle furnace 750~850 DEG C it is (specifically more It is few, or you in the range of float) heat preservation 5h；
8) is washed with deionized repeatedly, is collected by centrifugation by step 7) product B and molten salt mixture after furnace cooling, And with 0.1mol/L AgNO3Solution is detected to cannot find Cl?Ion, dry 6~12h, obtains faint yellow in 100 DEG C of baking ovens Sheet BaTiO3The brilliant product of micron.
The BaTiO of comparative example 23The XRD diagram of product is shown in Fig. 1, BaTiO in Fig. 13The position of each diffraction maximum and relative intensity are equal It matches with PDF card (PDF#76-0744), shows that product is tetragonal phase BaTiO3, but there are a small amount of raw materials to spread out in XRD spectrum Penetrate peak.

Claims (4)

1. a liang step molten-salt growth method prepares sheet BaTiO3 microns of brilliant method, which comprises the following steps:
Raw material: barium source raw material is using the pure BaCO of analysis3, titanium source raw material use Anatase TiO2；Fused salt auxiliary agent NaCl/KCl.
(1) the barium source raw material, titanium source raw material and fused salt auxiliary agent of metering are pressed BaCO by first step fused salt process3: TiO2: NaCl:KCl The mixing of=6.6:17:170:170 molar ratio；
(2) obtained mixture hand-ground is obtained into uniformed powder；
(3) obtained powder is placed in crucible, is placed in 950~1050 DEG C of calcining 5h in Muffle furnace, obtains calcined production The mixture of object A and fused salt；
(4) by the mixture furnace cooling of step (3) products therefrom and fused salt, drying is washed, Ba is obtained6Ti17O40Single-chip；
(5) second step fused salt process, by Ba obtained by step (4)6Ti17O40As titanium source and part barium source and barium source raw material, fused salt Auxiliary agent presses Ba6Ti17O40: BaCO3: the molar ratio 1:11:120:120 mixing of NaCl:KCl；
(6) obtained mixture hand-ground is obtained to uniformed powder；
(7) obtained powder is placed in crucible, is placed in Muffle furnace 750~1050 DEG C (preferably 1000-1050 DEG C) calcinings 5h obtains the mixture of calcined product B and fused salt；
(8) washing after calcined mixture furnace cooling is dried to obtain product B i.e. sheet BaTiO3Micron is brilliant.
2. two steps molten-salt growth method described in accordance with the claim 1 prepares sheet BaTiO3 microns of brilliant method, which is characterized in that Ba6Ti17O40Single-chip, a diameter of 5 microns to 15 microns, with a thickness of 0.4 to 0.7 micron.
3. two steps molten-salt growth method described in accordance with the claim 1 prepares sheet BaTiO3 microns of brilliant method, which is characterized in that sheet BaTiO3, a diameter of 6 microns to 19 microns, with a thickness of 0.9 to 1.3 micron.
4. two steps molten-salt growth method described in accordance with the claim 1 prepares sheet BaTiO3 microns of brilliant method, which is characterized in that step (7) temperature is 1000-1050 DEG C.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN117383928A (en) * 2023-01-29 2024-01-12 哈尔滨工业大学 Preparation method of <111> oriented barium titanate template with high yield and large diameter-thickness ratio
CN117383928B (en) * 2023-01-29 2024-05-10 哈尔滨工业大学 Preparation method of <111> oriented barium titanate template with high yield and large diameter-thickness ratio

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1962542A (en) * 2006-12-08 2007-05-16 清华大学 Micron level sheet-like barium titanate crystal and its preparation method
CN101531394A (en) * 2009-02-27 2009-09-16 同济大学 Method for preparing barium titanate powder
JP4752194B2 (en) * 2003-05-21 2011-08-17 旭硝子株式会社 Method for producing barium titanate fine particles
CN102276255A (en) * 2011-06-02 2011-12-14 西北工业大学 Preparation method for sheet-like barium titanate microcrystalline powder
CN104925856A (en) * 2015-07-07 2015-09-23 北京工业大学 Method for preparing BaTiO3 nanowire through two-step salt melting method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4752194B2 (en) * 2003-05-21 2011-08-17 旭硝子株式会社 Method for producing barium titanate fine particles
CN1962542A (en) * 2006-12-08 2007-05-16 清华大学 Micron level sheet-like barium titanate crystal and its preparation method
CN101531394A (en) * 2009-02-27 2009-09-16 同济大学 Method for preparing barium titanate powder
CN102276255A (en) * 2011-06-02 2011-12-14 西北工业大学 Preparation method for sheet-like barium titanate microcrystalline powder
CN104925856A (en) * 2015-07-07 2015-09-23 北京工业大学 Method for preparing BaTiO3 nanowire through two-step salt melting method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ASTRI BJØRNETUN HAUGEN ET AL.: "Effect of crystallographic orientation in textured Ba0.92Ca0.08TiO3 piezoelectric ceramics", 《JOURNAL OF APPLIED PHYSICS》 *
TOMOYA SATO ET AL.: "Preparation of <111>-textured BaTiO3 ceramics by templated grain growth method using novel template particles", 《CERAMICS INTERNATIONAL》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN117383928A (en) * 2023-01-29 2024-01-12 哈尔滨工业大学 Preparation method of <111> oriented barium titanate template with high yield and large diameter-thickness ratio
CN117383928B (en) * 2023-01-29 2024-05-10 哈尔滨工业大学 Preparation method of <111> oriented barium titanate template with high yield and large diameter-thickness ratio

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