CN103924300A - Preparation method of barium strontium titanate crystal whisker material - Google Patents
Preparation method of barium strontium titanate crystal whisker material Download PDFInfo
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- CN103924300A CN103924300A CN201410191657.0A CN201410191657A CN103924300A CN 103924300 A CN103924300 A CN 103924300A CN 201410191657 A CN201410191657 A CN 201410191657A CN 103924300 A CN103924300 A CN 103924300A
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Abstract
The invention discloses a preparation method of a barium strontium titanate crystal whisker material. The preparation method includes the steps that (1) barium acetate and strontium acetate are weighed and dissolved in glacial acetic acid, and an obtained solution is marked as a solution A; (2) butyl titanate is weighed and dissolved in absolute ethyl alcohol, and an obtained solution is marked as a solution B; (3) deionized water and ethylene glycol monomethyl ether are mixed, and an obtained solution is marked as a solution C; (4) the solution B and the solution C are led into the solution A slowly by the utilization of a glass rod; (5) the mixed solution is placed in a 60 DEG C constant-temperature water bath kettle, the temperature is kept for 1 h, and gel is obtained; (6) the dried gel is ground into gel powder with the grain size being 5-20 micrometers; (7) the gel powder is placed into a hydrothermal reaction kettle, and heat preservation is conducted on the gel powder at the temperature of 200-250 DEG C for 9-15 hours; (8) a product generated in the step (7) is washed, filtered and dried to obtain barium strontium titanate crystal whiskers. The preparation method is reliable in principle, simple in process, easy to operate and capable of preparing the barium strontium titanate crystal whisker material which has excellent electromagnetic property and mechanical property, and has broad market prospects.
Description
Technical field
The preparation method who the present invention relates to a kind of strontium-barium titanate crystal whisker materials, belongs to field of functional materials.
Background technology
Strontium-barium titanate (Ba
xsr
1-xtiO
30≤x≤1, be abbreviated as BST) be the Typical Representative of ferroelectric material, its cation constituent between strontium titanate and barium titanate between the two, the performances such as its specific inductivity and Curie temperature can change along with the adjusting of cation constituent, thereby it is a kind of excellent performance and the piezoelectric that is always subject to extensive concern.
Hydrothermal synthesis method, sol-gel method, pulsed laser deposition technique and the discharge plasma sintering method of adopting are prepared barium-strontium titanate powder and superfine powder more on the one hand now, apply on the other hand sol-gel method, radio-frequency magnetron sputter method etc. and prepare barium strontium titanate.Whisker is the one-dimensional material with certain length-to-diameter ratio growing into monocrystalline form, and its diameter is little, atom high-sequential.Strontium-barium titanate whisker, its crystal preferential growth, makes BST whisker have anisotropy, significant for the piezoelectric property that improves barium strontium titanate material.
The present invention adopts sol-gel method to prepare strontium-barium titanate presoma, then presoma is carried out to hydrothermal treatment consists, and then obtains strontium-barium titanate whisker.Wherein sol-gel method has simple to operate, the advantage such as low to requirement for experiment condition, composition is easy to control, do not introduce impurity substances, the presoma composition that obtains is even; Hydro-thermal reaction is compared with traditional sintering, and temperature of reaction is low, and reactant is uniformly dispersed in solution, and is attended by high pressure, so just may obtain the product that under atmospheric pressure cannot obtain.
Summary of the invention
The preparation method who the object of the present invention is to provide a kind of strontium-barium titanate crystal whisker materials, principle is reliable, and technique is simple, easy handling, can prepare the strontium-barium titanate crystal whisker materials with good electromagnetic performance and mechanical property, fill up the blank of prior art, there are wide market outlook.
For reaching above technical purpose, the invention provides following technical scheme.
The present invention adopts sol-gel method to prepare strontium-barium titanate xerogel as presoma, then presoma is adopted hydrothermal growth process to prepare strontium-barium titanate whisker, and concrete steps are as follows:
(1) take barium acetate CH
3cOO)
2ba and strontium acetate (CH
3cOO)
2sr0.5H
2o, making the mol ratio of Ba and Sr is 1:1, is dissolved in 40-100ml glacial acetic acid, total strength of solution is 0.8-2mol/L, with glass stick, constantly stirs, and adopts heating in water bath to accelerate dissolving in whipping process, is labeled as solution A;
(2) take butyl (tetra) titanate, making the mol ratio of Ti and Ba is 2:1, is dissolved in 40-100ml dehydrated alcohol, is labeled as solution B;
(3) measure 40-100ml deionized water and 20-50ml ethylene glycol monomethyl ether, both are mixed, be labeled as solution C;
(4) solution B is slowly drained in solution A with glass stick, with the continuous stirred solution A of magnetic stirring apparatus, solution C is slowly drained in the solution A that has added solution B with glass stick, equally with the continuous stirred solution A of magnetic stirring apparatus, after solution mixes, more than magnetic stirrer mixing solutions 1h, it is mixed;
(5) mixing solutions is put into the thermostat water bath of 60 ℃ and be incubated 1h left and right, obtain gel, then gel is put into 75 ℃ of dry 120h of loft drier;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5-20um, as hydro-thermal presoma;
(7) weigh 5-10g Gelatin powder and put into the hydrothermal reaction kettle that volume is 50ml, with 2mol/LKOH, as mineralizer, compactedness is controlled at 70-95%, and temperature of reaction kettle is controlled at 200-250 ℃ of left and right, and soaking time is 9-15h;
(8) (7) products therefrom is repeatedly cleaned with deionized water and dehydrated alcohol, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then with 625 order filter sieve, filter, the material after filtering is dry, obtain strontium-barium titanate whisker.
In preparation process, use be 316 stainless steel high temperature high-pressure hydrothermal reaction kettles, inner bag is bulk material.
In preparation process, the raw material of use is all commercially available chemical pure.
Compared with prior art, beneficial effect of the present invention is:
(1) the present invention adopts the preparation method that sol-gel method is combined with Hydrothermal Synthesis growth method, utilizes respectively advantage separately, and the mode that adopts this multiple preparation method to combine is prepared the type material being not easy to obtain.
(2) the strontium-barium titanate whisker of preparing, radical length 100～500um, axially diameter is 0.5～5um, length-to-diameter ratio is 50～200, can utilize its anisotropy as functional materials, especially as electronic material, uses.
(3) the strontium-barium titanate whisker of preparing, can utilize its mechanical property to use as strengthening toughening composition.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the strontium-barium titanate whisker prepared of the present invention.
Fig. 2 is the SEM figure of the strontium-barium titanate whisker prepared of the present invention.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention, but all embodiment are not construed as limiting the invention.
Embodiment 1
(1) weigh 10.2169g (CH
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), is then dissolved in the two 80ml glacial acetic acid, and strength of solution is 1mol/L, with glass stick, constantly stirs, and adopts heating in water bath to accelerate dissolving in whipping process, is labeled as solution A;
(2) weigh 27.2289g butyl (tetra) titanate (mol ratio of Ti and Ba is 2:1), be dissolved in 80ml dehydrated alcohol, be labeled as solution B;
(3) measure 80ml deionized water and 40ml ethylene glycol monomethyl ether, both are mixed, be labeled as solution C;
(4) complete soln B is slowly drained in solution A with glass stick, with magnetic stirring apparatus stirred solution A constantly, complete soln C is slowly drained in the solution A that has added solution B with glass stick, equally with magnetic stirring apparatus stirred solution A constantly, after solution mixes, more than magnetic stirrer mixing solutions 1h, it is mixed;
(5) mixing solutions is put into the thermostat water bath of 60 ℃ and be incubated 1h left and right, obtain gel, then gel is put into 75 ℃ of dry 120h of loft drier;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5～20um, as hydro-thermal presoma;
(7) weigh 5g Gelatin powder and put into the hydrothermal reaction kettle that volume is 50ml, with the KOH of 2mol/L, as mineralizer, the compactedness of reactor is 80%, and temperature of reaction kettle is 230 ℃, and soaking time is 12h;
(8) product of step (7) is taken out, with deionized water and dehydrated alcohol, repeatedly clean, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then with 625 object filter sieve, filter, material after filtering is dry, obtain strontium-barium titanate whisker.
Fig. 1 is the XRD figure of the strontium-barium titanate whisker of embodiment 1 preparation.From figure, can draw, its angle of diffraction is consistent with the angle of diffraction of standard card #39-1395, and its (110) face diffracted intensity is very large, and each diffraction peak is all very sharp-pointed.
Fig. 2 is the SEM figure of the strontium-barium titanate whisker of embodiment 1 preparation.As can be seen from the figure, whisker radical length is between 100～300um, and axially diameter is 1～5um, and length-to-diameter ratio is between 30～100.
Embodiment 2
(1) weigh 10.2169g (CH
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), is then dissolved in the two 80ml glacial acetic acid, and strength of solution is 1mol/L, with glass stick, constantly stirs, and adopts heating in water bath to accelerate dissolving in whipping process, is labeled as solution A;
(2) weigh 27.2289g butyl (tetra) titanate (mol ratio of Ti and Ba is 2:1), be dissolved in 80ml dehydrated alcohol, be labeled as solution B;
(3) measure 80ml deionized water and 40ml ethylene glycol monomethyl ether, both are mixed, be labeled as solution C;
(4) complete soln B is slowly drained in solution A with glass stick, with magnetic stirring apparatus stirred solution A constantly, complete soln C is slowly drained in the solution A that has added solution B with glass stick, equally with magnetic stirring apparatus stirred solution A constantly, more than magnetic stirrer mixing solutions 1h, it is mixed;
(5) mixing solutions is put into the thermostat water bath of 60 ℃ and be incubated 1h left and right, obtain gel, then gel is put into 75 ℃ of dry 120h of loft drier;
(6) gel of drying is taken out, grind to form the Gelatin powder of 5～20um, as hydro-thermal presoma;
(7) weigh 5g Gelatin powder and put into the hydrothermal reaction kettle that volume is 50ml, with the KOH of 2mol/L, as mineralizer, the compactedness of reactor is 85%, and temperature of reaction kettle is 230 ℃, and soaking time is 12h;
(8) product of step (7) is taken out, with deionized water and dehydrated alcohol, repeatedly clean, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then with 625 object filter sieve, filter, material after filtering is dry, obtain strontium-barium titanate whisker.
Embodiment 3
(1) weigh 10.2169g (CH
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), is then dissolved in the two 80ml glacial acetic acid, and strength of solution is 1mol/L, with glass stick, constantly stirs, and adopts heating in water bath to accelerate dissolving in whipping process, is labeled as solution A;
(2) weigh 27.2289g butyl (tetra) titanate (mol ratio of Ti and Ba is 2:1), be then dissolved in 80ml dehydrated alcohol, be labeled as solution B;
(3) measure 80ml deionized water and 40ml ethylene glycol monomethyl ether, both are mixed, be labeled as solution C;
(4) solution B is slowly drained in solution A with glass stick, with magnetic stirring apparatus stirred solution A constantly, solution C is slowly drained in solution A with glass stick, equally with magnetic stirring apparatus stirred solution A constantly, after solution mixes, more than magnetic stirrer mixing solutions 1h, it is mixed;
(5) mixing solutions is put into the thermostat water bath of 60 ℃ and be incubated 1h left and right, obtain gel, then gel is put into 75 ℃ of dry 120h of loft drier;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5～20um, as hydro-thermal presoma;
(7) weigh 5g Gelatin powder and put into the hydrothermal reaction kettle that volume is 50ml, with the KOH of 2mol/L, as mineralizer, the compactedness of reactor is 90%, and temperature of reaction kettle is 230 ℃, and soaking time is 12h;
(8) product of step (7) is taken out, with deionized water and dehydrated alcohol, repeatedly clean, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then with 625 object filter sieve, filter, material after filtering is dry, obtain strontium-barium titanate whisker.
Claims (1)
1. a preparation method for strontium-barium titanate crystal whisker materials, comprises the following steps successively:
(1) take barium acetate CH
3cOO)
2ba and strontium acetate (CH
3cOO)
2sr0.5H
2o, making the mol ratio of Ba and Sr is 1:1, is dissolved in 40-100ml glacial acetic acid, total strength of solution is 0.8-2mol/L, is labeled as solution A;
(2) take butyl (tetra) titanate, making the mol ratio of Ti and Ba is 2:1, is dissolved in 40-100ml dehydrated alcohol, is labeled as solution B;
(3) measure 40-100ml deionized water and 20-50ml ethylene glycol monomethyl ether, both are mixed, be labeled as solution C;
(4) solution B is slowly drained in solution A with glass stick, solution C is slowly drained in the solution A that has added solution B with glass stick, use magnetic stirrer mixing solutions, it is mixed;
(5) mixing solutions is put into the thermostat water bath of 60 ℃ and be incubated 1h left and right, obtain gel;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5-20um;
(7) weigh 5-10g Gelatin powder and put into hydrothermal reaction kettle, with 2mol/LKOH, as mineralizer, compactedness is controlled at 70-95%, and temperature of reaction kettle is controlled at 200-250 ℃ of left and right, and soaking time is 9-15h;
(8) (7) products therefrom is cleaned with deionized water and dehydrated alcohol, then use ultrasonic oscillation, then with 625 order filter sieve, filter, the material after filtering is dry, obtain strontium-barium titanate whisker.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757351A (en) * | 2016-11-18 | 2017-05-31 | 西南石油大学 | A kind of preparation method of barium strontium titanate crystal beam material |
| CN114293258A (en) * | 2021-12-10 | 2022-04-08 | 南京航空航天大学 | Barium dititanate doped micro powder and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311376A (en) * | 2008-02-26 | 2008-11-26 | 浙江大学 | Method for preparing strontium titanate nanometer powder of one-dimensional structure |
| 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 |
| CN102691105A (en) * | 2012-06-12 | 2012-09-26 | 浙江大学 | Method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311376A (en) * | 2008-02-26 | 2008-11-26 | 浙江大学 | Method for preparing strontium titanate nanometer powder of one-dimensional structure |
| 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 |
| CN102691105A (en) * | 2012-06-12 | 2012-09-26 | 浙江大学 | Method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757351A (en) * | 2016-11-18 | 2017-05-31 | 西南石油大学 | A kind of preparation method of barium strontium titanate crystal beam material |
| CN114293258A (en) * | 2021-12-10 | 2022-04-08 | 南京航空航天大学 | Barium dititanate doped micro powder and preparation method and application thereof |
| CN114293258B (en) * | 2021-12-10 | 2023-01-03 | 南京航空航天大学 | Barium dititanate doped micro powder and preparation method and application thereof |
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