CN103924300B - A kind of preparation method of strontium-barium titanate crystal whisker materials - Google Patents
A kind of preparation method of strontium-barium titanate crystal whisker materials Download PDFInfo
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- CN103924300B CN103924300B CN201410191657.0A CN201410191657A CN103924300B CN 103924300 B CN103924300 B CN 103924300B CN 201410191657 A CN201410191657 A CN 201410191657A CN 103924300 B CN103924300 B CN 103924300B
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Abstract
The invention discloses a kind of preparation method of strontium-barium titanate crystal whisker materials, comprising: (1) takes barium acetate and strontium acetate is dissolved in glacial acetic acid, is labeled as solution A; (2) taking butyl (tetra) titanate is dissolved in dehydrated alcohol, is labeled as solution B; (3) deionized water and ethylene glycol monomethyl ether mixing, be labeled as solution C; (4) solution B and solution C glass stick are slowly drained in solution A; (5) mixing solutions is put into 60 DEG C of thermostat water baths and be incubated 1h, obtain gel; (6) particle diameter is become by the gel abrasive of oven dry to be the Gelatin powder of 5-20um; (7) Gelatin powder is put into hydrothermal reaction kettle, at 200-250 DEG C, be incubated 9-15h; (8) by the cleaning of (7) products therefrom, filtration, drying, strontium-barium titanate whisker is obtained.The principle of the invention is reliable, and technique is simple, and easy handling, can prepare the strontium-barium titanate crystal whisker materials with excellent electromagnetic performance and mechanical property, have wide market outlook.
Description
Technical field
The present invention relates to a kind of preparation method of strontium-barium titanate crystal whisker materials, belong 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 adjustment of cation constituent, and thus it is a kind of excellent performance and is subject to the piezoelectric of extensive concern always.
Present one side adopts hydrothermal synthesis method, sol-gel method, pulsed laser deposition technique and discharge plasma sintering method to prepare barium-strontium titanate powder and superfine powder more, and applying sol-gel method, radio-frequency magnetron sputter method etc. prepares barium strontium titanate on the other hand.Whisker is the one-dimensional material with certain length-to-diameter ratio grown into single crystal form, and its diameter is little, and atom high is orderly.Strontium-barium titanate whisker, its crystal preferential growth, makes BST whisker have anisotropy, significant for the piezoelectric property improving barium strontium titanate material.
The present invention adopts sol-gel method to prepare strontium-barium titanate presoma, then presoma is carried out hydrothermal treatment consists, and then obtains strontium-barium titanate whisker.Wherein sol-gel method has simple to operate, low to requirement for experiment condition, the advantage such as composition is easy to control, do not introduce impurity substances, presoma uniform composition of obtaining; Hydro-thermal reaction is compared with traditional sintering, and temperature of reaction is low, and reactant is uniformly dispersed in the solution, and is attended by high pressure, so just may obtain the product that under atmospheric pressure cannot obtain.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of strontium-barium titanate crystal whisker materials, principle is reliable, and technique is simple, easy handling, the strontium-barium titanate crystal whisker materials with excellent electromagnetic performance and mechanical property can be prepared, filled 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, and then adopted by presoma hydrothermal growth process to prepare strontium-barium titanate whisker, concrete steps are as follows:
(1) barium acetate (CH is taken
3cOO)
2ba and strontium acetate (CH
3cOO)
2sr0.5H
2o, the mol ratio making Ba and Sr is 1:1, and be dissolved in 40-100ml glacial acetic acid, total strength of solution is 0.8-2mol/L, constantly stirs with glass stick, adopts heating in water bath to accelerate to dissolve, be labeled as solution A in whipping process;
(2) take butyl (tetra) titanate, the mol ratio making 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, is labeled as solution C;
(4) solution B glass stick is slowly drained in solution A, with the continuous stirred solution A of magnetic stirring apparatus, solution C glass stick is slowly drained into and has added in the solution A of solution B, the continuous stirred solution A of same magnetic stirring apparatus, after solution mixing, with magnetic stirrer more than mixing solutions 1h, it is made to mix;
(5) thermostat water bath mixing solutions being put into 60 DEG C is incubated 1h, obtains gel, then gel is put into loft drier 75 DEG C of dry 120h;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5-20 μm, 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 controls 70-95%, and temperature of reaction kettle controls at 200-250 DEG C, and soaking time is 9-15h;
(8) (7) products therefrom deionized water and dehydrated alcohol are repeatedly cleaned, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then filter with 625 order filter sieve, by dry for the material after filtering, obtain strontium-barium titanate whisker.
In preparation process, use 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 respective advantage respectively, and the mode adopting this multiple preparation method to combine prepares the type material be not easy to obtain.
(2) the strontium-barium titanate whisker prepared, radical length 100 ~ 500 μm, axial diameter is 0.5 ~ 5 μm, and length-to-diameter ratio is 50 ~ 200, its anisotropy can be utilized as functional materials, especially use as electronic material.
(3) the strontium-barium titanate whisker prepared, can utilize its mechanical property to use as activeness and quietness matrix material.
Accompanying drawing explanation
Fig. 1 is the XRD figure of strontium-barium titanate whisker prepared by the present invention.
Fig. 2 is the SEM figure of strontium-barium titanate whisker prepared by the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but all embodiments are not construed as limiting the invention.
Embodiment 1
(1) 10.2169g (CH is weighed
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), then the two is dissolved in 80ml glacial acetic acid, strength of solution is 1mol/L, constantly stirs with glass stick, adopts heating in water bath to accelerate to dissolve, be labeled as solution A in whipping process;
(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, is labeled as solution C;
(4) complete soln B glass stick is slowly drained in solution A, with magnetic stirring apparatus constantly stirred solution A, complete soln C glass stick is slowly drained into and has added in the solution A of solution B, equally with magnetic stirring apparatus constantly stirred solution A, after solution mixing, with magnetic stirrer more than mixing solutions 1h, it is made to mix;
(5) thermostat water bath mixing solutions being put into 60 DEG C is incubated 1h, obtains gel, then gel is put into loft drier 75 DEG C of dry 120h;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5 ~ 20 μm, 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 DEG C, and soaking time is 12h;
(8) product of step (7) is taken out, repeatedly clean with deionized water and dehydrated alcohol, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then filter with 625 object filter sieve, by dry for the material after filtering, obtain strontium-barium titanate whisker.
Fig. 1 is the XRD figure of strontium-barium titanate whisker prepared by embodiment 1.Can draw from figure, 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 strontium-barium titanate whisker prepared by embodiment 1.As can be seen from the figure, whisker radical length is between 100 ~ 300 μm, and axial diameter is 1 ~ 5 μm, and length-to-diameter ratio is between 30 ~ 100.
Embodiment 2
(1) 10.2169g (CH is weighed
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), then the two is dissolved in 80ml glacial acetic acid, strength of solution is 1mol/L, constantly stirs with glass stick, adopts heating in water bath to accelerate to dissolve, be labeled as solution A in whipping process;
(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, is labeled as solution C;
(4) complete soln B glass stick is slowly drained in solution A, with magnetic stirring apparatus constantly stirred solution A, complete soln C glass stick is slowly drained into and has added in the solution A of solution B, equally with magnetic stirring apparatus constantly stirred solution A, with magnetic stirrer more than mixing solutions 1h, it is made to mix;
(5) thermostat water bath mixing solutions being put into 60 DEG C is incubated 1h, obtains gel, then gel is put into loft drier 75 DEG C of dry 120h;
(6) gel of drying is taken out, grind to form the Gelatin powder of 5 ~ 20 μm, 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 DEG C, and soaking time is 12h;
(8) product of step (7) is taken out, repeatedly clean with deionized water and dehydrated alcohol, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then filter with 625 object filter sieve, by dry for the material after filtering, obtain strontium-barium titanate whisker.
Embodiment 3
(1) 10.2169g (CH is weighed
3cOO)
2ba, 8.5894g (CH
3cOO)
2sr0.5H
2o (mol ratio of Ba and Sr is 1:1), then the two is dissolved in 80ml glacial acetic acid, strength of solution is 1mol/L, constantly stirs with glass stick, adopts heating in water bath to accelerate to dissolve, be labeled as solution A in whipping process;
(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, is labeled as solution C;
(4) solution B glass stick is slowly drained in solution A, with magnetic stirring apparatus constantly stirred solution A, solution C glass stick is slowly drained in solution A, equally with magnetic stirring apparatus constantly stirred solution A, after solution mixing, with magnetic stirrer more than mixing solutions 1h, it is made to mix;
(5) thermostat water bath mixing solutions being put into 60 DEG C is incubated 1h, obtains gel, then gel is put into loft drier 75 DEG C of dry 120h;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5 ~ 20 μm, 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 DEG C, and soaking time is 12h;
(8) product of step (7) is taken out, repeatedly clean with deionized water and dehydrated alcohol, with ultrasonic oscillation, whisker and powder, powder and powder, whisker and whisker are disperseed again, then filter with 625 object filter sieve, by dry for the material after filtering, obtain strontium-barium titanate whisker.
Claims (1)
1. a preparation method for strontium-barium titanate crystal whisker materials, comprises the following steps successively:
(1) barium acetate (CH is taken
3cOO)
2ba and strontium acetate (CH
3cOO)
2sr0.5H
2o, the mol ratio making Ba and Sr is 1:1, and be 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, the mol ratio making 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, is labeled as solution C;
(4) solution B glass stick is slowly drained in solution A, solution C glass stick is slowly drained into and has added in the solution A of solution B, use magnetic stirrer mixing solutions, make it mix;
(5) thermostat water bath mixing solutions being put into 60 DEG C is incubated 1h, obtains gel, then gel is put into loft drier 75 DEG C of dry 120h;
(6) gel of drying is taken out, grind to form the Gelatin powder that particle diameter is 5-20 μm;
(7) weigh 5-10g Gelatin powder and put into hydrothermal reaction kettle, with 2mol/LKOH as mineralizer, compactedness controls 70-95%, and temperature of reaction kettle controls at 200-250 DEG C, and soaking time is 9-15h;
(8) by (7) products therefrom deionized water and washes of absolute alcohol, then use ultrasonic oscillation, then filter with 625 order filter sieve, by dry for the material after filtering, obtain strontium-barium titanate whisker.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| 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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