CN106757351A - A kind of preparation method of barium strontium titanate crystal beam material - Google Patents
A kind of preparation method of barium strontium titanate crystal beam material Download PDFInfo
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- CN106757351A CN106757351A CN201611018862.2A CN201611018862A CN106757351A CN 106757351 A CN106757351 A CN 106757351A CN 201611018862 A CN201611018862 A CN 201611018862A CN 106757351 A CN106757351 A CN 106757351A
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- barium
- strontium
- crystal beam
- beam material
- strontium titanate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a kind of preparation method of barium strontium titanate crystal beam material, including：1) butyl titanate is mixed with the deionized water of excess, obtains suspension；2) by barium acetate and strontium acetate deionized water dissolving, the strontium barium aqueous solution is obtained；3) the strontium barium aqueous solution is added dropwise in suspension, is precipitated；4) after precipitation is through filtering, cleaning, 24h is dried at 70 DEG C；5) dried depositing abrasive is dispersed into fine particle, is put into hydrothermal reaction kettle, add NaOH solution, sealed after stirring, at 160 200 DEG C, soaking time is 16 24h to temperature of reaction kettle；6) hydrothermal product is taken out, is cleaned with deionized water, and disperse product with dispersant and ultrasonic oscillation device, then filtered with 625 mesh filter screens, obtain barium strontium titanate crystal beam material.Principle of the invention reliability, process is simple, it is easy to operate, can prepare the barium strontium titanate crystal beam material with excellent electromagnetic performance and mechanical property.
Description
Technical field
The present invention relates to a kind of preparation method of barium strontium titanate crystal beam material, belong to field of functional materials.
Background technology
Barium strontium titanate (BaxSr1-xTiO3, abbreviation BST) and it is by BaTiO3With SrTiO3The solid solution of formation.It not only has
High-k, low-dielectric loss, Curie temperature with composition change and dielectric constant with electric field nonlinear change the features such as,
And with good chemical stability, heat endurance and insulating properties.BST materials are a kind of widely used thermo-sensitive material, electricity
Container material and ferroelectric piezoelectric material, as one of most widely studied material in integrated device field.
The electric property of barium strontium titanate material is closely related with the microstructure of material such as crystallite dimension and crystal habit, brilliant
Better, material has excellent physical and chemical performance to the thinner and fine and close BST dielectric materials characteristic higher of grain, industrially widely should
Obvious to all with being worth, with the development of increasingly mature microelectronic industry, people more and more pay attention to and pay close attention to BST ceramics
Material.
Now concerning the research of barium strontium titanate material, the direction of superfines, film and doping, the system of use are concentrated on
Preparation Method has hydrothermal synthesis method, sol-gal process, pulsed laser deposition technique, radio-frequency magnetron sputter method and plasma discharging to burn
Knot etc., and the research of the orientation of growth and crystal habit for barium strontium titanate crystal is also few.And dimension is to determine nano material
One of key factor of property, therefore, the control for the size and dimension of material is extremely important.Compared with the control of size,
Pattern control to crystal is a problem being more difficult to.Barium strontium titanate crystal beam is the result of preferred orientation growth, with excellent
Anisotropy, the piezoelectricity etc. for improving barium strontium titanate material is significant, while more one-dimensional whisker is easier to life
Grow up to big flaky material, this problem is aligned so as to solve whisker.
The present invention prepares barium strontium titanate presoma using coprecipitation, presoma then is carried out into hydro-thermal process, and then obtain
To one-dimensional barium strontium titanate crystal beam.Wherein coprecipitation has simple to operate, low to experiment condition requirement, composition easy to control, no
The advantages of introducing impurity substances；Hydro-thermal reaction is compared with traditional sintering, and reaction temperature is low, and reactant disperses in the solution
It is even, and with high pressure, thus it is likely to be obtained the product that cannot be obtained under atmospheric pressure.
The content of the invention
It is an object of the invention to provide a kind of preparation method of barium strontium titanate crystal beam material, the method principle reliability,
Process is simple, it is easy to operate, can prepare the barium strontium titanate crystal beam material with excellent electromagnetic performance and mechanical property.
To reach above technical purpose, the present invention uses following technical scheme.
The present invention prepares the co-precipitate containing anatase phase as presoma using coprecipitation, then by forerunner
Body prepares barium strontium titanate crystal beam using hydrothermal growth process.
A kind of preparation method of barium strontium titanate crystal beam material, comprises the following steps successively：
1) butyl titanate is weighed, it is mixed with excessive deionized water, the mol ratio of control water and butyl titanate is in 40-
60：Between 1, suspension is obtained；
2) barium acetate and strontium acetate are weighed, the mol ratio for making barium and strontium is 1:1, the mol ratio of titanium and barium is 2:1, and spend
Ion water dissolves, obtain the strontium barium aqueous solution, and total solution concentration is 0.8-2mol/L；
3) the strontium barium aqueous solution is added dropwise in suspension, during dropwise addition, is stirred continuously suspension, sunk
Form sediment；
4) precipitation dries 24h, as hydro-thermal presoma by filtering, and after being cleaned with deionized water at 70 DEG C；
5) dried depositing abrasive is dispersed into fine particle, weighs 3-5g and be put into the hydrothermal reaction kettle that volume is 50ml
In, the NaOH solution of 2mol/L is subsequently adding as mineralizer, compactedness is controlled between 70-90%, stirs equal with glass bar
After even, seal, temperature of reaction kettle is controlled at 160-200 DEG C or so, and soaking time is 16-24h；
6) reaction terminate, take out hydrothermal product, clean with deionized water repeatedly, and with calgon as dispersant with
Ultrasonic oscillation device disperses product, is then filtered using 625 mesh filter screens, removes unnecessary powder, obtains relatively pure titanium
Sour strontium crystal of barium beam material.
In preparation process of the present invention, the HTHP hydro-thermal reaction kettle for using material to be made for 316L stainless steels.
In preparation process of the present invention, the raw material for using all is that commercially available chemistry is pure.
Compared with prior art, the beneficial effects of the present invention are：
(1) the barium strontium titanate crystal beam prepared has excellent anisotropy, and it is fixed that crystal beam is more easily implemented than whisker
To arrangement, it is easy to commercialization；
(2) preparation method prepares presoma using coprecipitation, and method is simple, and easy to operate, easy to control, cost is relatively low, together
When avoid generate interphase；
(3) preparation method that the present invention is combined using coprecipitation with Hydrothermal Synthesiss growth method, is utilized respectively its respective
Advantage, the research of the current many materials in this area is all combined to realize with preparation using various preparation methods.
Brief description of the drawings
Fig. 1 is the XRD of the coprecipitated product that the present invention is obtained.
Fig. 2 is the SEM figures of the coprecipitated product that the present invention is obtained.
Fig. 3 is the XRD of the barium strontium titanate crystal beam that the present invention is obtained.
Fig. 4 is the SEM figures of the barium strontium titanate crystal beam that the present invention is obtained.
Specific embodiment
With reference to embodiments the present invention is further illustrated with accompanying drawing.
Embodiment 1
1) weigh 27.2289g butyl titanates (0.08mol), then measure 60ml deionization add butyl titanate in, and
It is stirred continuously, obtains suspension；
2) barium acetate (0.04mol) of 10.2169g and the strontium acetate (0.04mol) of 8.5894g are weighed, and with 40ml's
Deionized water dissolving, obtains the strontium barium aqueous solution；
3) the strontium barium aqueous solution is added dropwise in suspension, it is outstanding using magnetic stirrer during dropwise addition
Supernatant liquid, mixing speed is 100r/min, stirs 30min, is co-precipitated；
4) precipitation is filtered using slow filter paper, is then cleaned with deionized water, refiltered, be repeated twice, 70 will be deposited in
24h is dried at DEG C, used as hydro-thermal presoma, Fig. 1 is the XRD of precipitation to product, and Fig. 2 is the SEM figures of precipitation；
5) presoma grinds to form particle diameter for 5~20um powder, weighs 5g and is put into the inner liner of reaction kettle that volume is 50ml, so
The NaOH solution 45ml of 2mol/L is added afterwards, after being stirred with glass bar, is sealed；
6) reactor is heated to 200 DEG C, is incubated 16h；
7) reaction terminates, and takes out hydrothermal product, is cleaned with deionized water repeatedly, and uses dispersant and ultrasonic oscillation device
Disperse product, then filtered using 625 mesh filter screens, remove unnecessary powder, obtain relatively pure crystal beam, crystal beam
Thing phase XRD is shown in Fig. 3, and microscopic appearance is as shown in Figure 4.
Fig. 1 is the XRD of the coprecipitated product that the present invention is obtained, and has various crystalline phases, wherein anatase TiO in figure2It is main
One of crystalline phase, angle and the angle of diffraction of standard card #21-1272 of diffraction maximum match.
Fig. 2 is the SEM figures of the co-precipitation in the present invention, can be clearly observed from figure and flock together and be orientated row
The consistent crystal beam of row, 100~400nm, a diameter of 20~80nm long.
Fig. 3 is the XRD of barium strontium titanate crystal beam that the present invention is obtained, and can be drawn from figure, its angle of diffraction and mark
The angle of diffraction of quasi- card #39-1395 is consistent, and its (110) face diffracted intensity is very big, and each diffraction maximum is all very sharp.
Fig. 4 is the SEM figures of the barium strontium titanate crystal beam that the present invention is obtained, it can be seen that crystal beam radical length
Between 50~300um, axial a diameter of 4~8um, draw ratio between 10~50, a branch of crystal of root containing 10-100.
Embodiment 2
1) weigh 27.2289g butyl titanates (0.08mol), then measure 72ml deionization add butyl titanate in, and
It is stirred continuously, obtains suspension；
2) barium acetate (0.04mol) of 10.2169g and the strontium acetate (0.04mol) of 8.5894g are weighed, and with 80ml's
Deionized water dissolving, obtains the strontium barium aqueous solution；
3) the strontium barium aqueous solution is added dropwise in suspension, it is outstanding using magnetic stirrer during dropwise addition
Supernatant liquid, mixing speed is 100r/min, stirs 30min, is co-precipitated；
4) precipitation is filtered using slow filter paper, is then cleaned with deionized water, refiltered, be repeated twice, 70 will be deposited in
24h is dried at DEG C, product is used as hydro-thermal presoma；
5) presoma grinds to form particle diameter for 5~20um powder, weighs 5g and is put into the inner liner of reaction kettle that volume is 50ml, so
The NaOH solution 40ml of 2mol/L is added afterwards, after being stirred with glass bar, is sealed；
6) reactor is heated to 180 DEG C, is incubated 20h；
7) reaction terminates, and takes out hydrothermal product, is cleaned with deionized water repeatedly, and uses dispersant and ultrasonic oscillation device
Disperse product, then filtered using 625 mesh filter screens, remove unnecessary powder, obtain relatively pure crystal beam.
Embodiment 3
1) weigh 27.2289g butyl titanates (0.08mol), then measure 86ml deionized water add Butyl Phthalate in,
And be stirred continuously, obtain suspension；
2) barium acetate (0.04mol) of 10.2169g and the strontium acetate (0.04mol) of 8.5894g are weighed, and with 100ml's
Deionized water dissolving, obtains the strontium barium aqueous solution；
3) the strontium barium aqueous solution is added dropwise in suspension, it is outstanding using magnetic stirrer during dropwise addition
Supernatant liquid, mixing speed is 100r/min, stirs 30min, is co-precipitated；
4) precipitation is filtered using slow filter paper, is then cleaned with deionized water, refiltered, be repeated twice, 70 will be deposited in
24h is dried at DEG C, product is used as hydro-thermal presoma；
5) presoma grinds to form particle diameter for 5~20um powder, weighs 5g and is put into the inner liner of reaction kettle that volume is 50ml, so
The NaOH solution 40ml of 2mol/L is added afterwards, after being stirred with glass bar, is sealed；
6) reactor is heated to 200 DEG C, is incubated 24h；
7) reaction terminates, and takes out hydrothermal product, is cleaned with deionized water repeatedly, and uses dispersant and ultrasonic oscillation device
Disperse product, then filtered using 625 mesh filter screens, remove unnecessary powder, obtain relatively pure crystal beam.
Claims (3)
1. a kind of preparation method of barium strontium titanate crystal beam material, comprises the following steps successively：
1) butyl titanate is weighed, it is mixed with excessive deionized water, the mol ratio of control water and butyl titanate is in 40-60：1
Between, obtain suspension；
2) barium acetate and strontium acetate are weighed, the mol ratio for making barium and strontium is 1:1, the mol ratio of titanium and barium is 2:1, and use deionization
Water dissolves, obtain the strontium barium aqueous solution, and total solution concentration is 0.8-2mol/L；
3) the strontium barium aqueous solution is added dropwise in suspension, during dropwise addition, is stirred continuously suspension, be precipitated；
4) precipitation dries 24h, as hydro-thermal presoma by filtering, and after being cleaned with deionized water at 70 DEG C；
5) dried depositing abrasive is dispersed into fine particle, weighs 3-5g and be put into hydrothermal reaction kettle, be subsequently adding 2mol/
The NaOH solution of L is controlled between 70-90%, after being stirred with glass bar, sealed, instead as mineralizer, compactedness
Answer kettle temperature control at 160-200 DEG C or so, soaking time is 16-24h；
6) reaction terminates, and takes out hydrothermal product, is cleaned with deionized water, and makes product point with dispersant and ultrasonic oscillation device
Dissipate, then filtered using 625 mesh filter screens, obtain barium strontium titanate crystal beam material.
2. a kind of preparation method of barium strontium titanate crystal beam material as claimed in claim 1, it is characterised in that the step 5)
Middle that dried depositing abrasive is dispersed into fine particle, the particle diameter of the fine particle is 5~20um.
3. a kind of preparation method of barium strontium titanate crystal beam material as claimed in claim 1, it is characterised in that the step 6)
Middle dispersant is calgon.
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Citations (6)
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|---|---|---|---|---|
| CN1670267A (en) * | 2005-01-12 | 2005-09-21 | 中国科学院新疆理化技术研究所 | Microwave hydrothermal synthesis method for nanometer crystal strontium titanate barium |
| CN101786654A (en) * | 2010-03-04 | 2010-07-28 | 西北工业大学 | Method for preparing nanometer barium-strontium titanate powder |
| CN101786887A (en) * | 2010-03-11 | 2010-07-28 | 西北工业大学 | Method for preparing nano barium-strontium titanate powder by adopting hydrothermal method |
| CN102515263A (en) * | 2011-12-29 | 2012-06-27 | 洛阳理工学院 | Preparation method of barium strontium titanate stellar crystal |
| CN103523824A (en) * | 2013-10-18 | 2014-01-22 | 上海电力学院 | Preparation method of nano flaky ferroelectric material for photocatalysis |
| CN103924300A (en) * | 2014-05-07 | 2014-07-16 | 西南石油大学 | Preparation method of barium strontium titanate crystal whisker material |
-
2016
- 2016-11-18 CN CN201611018862.2A patent/CN106757351A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1670267A (en) * | 2005-01-12 | 2005-09-21 | 中国科学院新疆理化技术研究所 | Microwave hydrothermal synthesis method for nanometer crystal strontium titanate barium |
| CN101786654A (en) * | 2010-03-04 | 2010-07-28 | 西北工业大学 | Method for preparing nanometer barium-strontium titanate powder |
| CN101786887A (en) * | 2010-03-11 | 2010-07-28 | 西北工业大学 | Method for preparing nano barium-strontium titanate powder by adopting hydrothermal method |
| CN102515263A (en) * | 2011-12-29 | 2012-06-27 | 洛阳理工学院 | Preparation method of barium strontium titanate stellar crystal |
| CN103523824A (en) * | 2013-10-18 | 2014-01-22 | 上海电力学院 | Preparation method of nano flaky ferroelectric material for photocatalysis |
| CN103924300A (en) * | 2014-05-07 | 2014-07-16 | 西南石油大学 | Preparation method of barium strontium titanate crystal whisker material |
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