CN102887705B - Preparation method of tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal - Google Patents
Preparation method of tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal Download PDFInfo
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- CN102887705B CN102887705B CN 201210409044 CN201210409044A CN102887705B CN 102887705 B CN102887705 B CN 102887705B CN 201210409044 CN201210409044 CN 201210409044 CN 201210409044 A CN201210409044 A CN 201210409044A CN 102887705 B CN102887705 B CN 102887705B
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- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 25
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002159 nanocrystal Substances 0.000 title abstract 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 54
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 31
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 229910052788 barium Inorganic materials 0.000 claims description 10
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- 239000003352 sequestering agent Substances 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 230000001143 conditioned effect Effects 0.000 claims description 5
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000003252 repetitive effect Effects 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000003990 capacitor Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- -1 sensors Substances 0.000 abstract 1
- 239000011232 storage material Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal. The preparation method comprises the following steps of: using barium acetate and tetrabutyl titanate as raw materials, adding deionized water, adding potassium hydroxide of an appropriate amount to promote crystallization, and carrying out hydrothermal reaction at the temperature of 110-240 DEG C so as to prepare the tetragonal-phase barium titanate (BaTiO3) hollow nanocrystal. The preparation method is simple in technical process, easy in control, low in cost and easy in scale production. The prepared product is high in purity, good in crystallinity, good in dispersivity and narrow in particle size distribution. The product has wide application prospects in the fields of microelectronic devices, high-capacity capacitors, sensors, storage materials, piezoelectric ceramics, filters and the like.
Description
Technical field
The present invention relates to the nanocrystalline preparation method of a kind of tetragonal-phase barium titanate hollow, belong to field of inorganic nonmetallic material.
Background technology
The performance of functional materials depends on their pattern, size and degree of crystallinity to a great extent, and the control of microscopic appearance has very large value to the utilization of material.Nano material has the physicochemical property more excellent than block materials, and the progress of science and technology and the miniaturization of electron device, and the nanometer of material has also been proposed to increasing requirement.Therefore, the preparation of control appearance of nano material becomes the focus that Materials science is paid close attention to and studied in recent years.
Barium titanate BaTiO
3a kind of widely used ferroelectric, piezoceramic material, mainly for the production of the electronic devices and components such as ceramic condenser of high dielectric.In recent years along with the development of laminated ceramic capacitor, to BaTiO
3the performance requriements of powder improves, and demand increases.Facts have proved, realize BaTiO
3high-purity, even, nanometer be to improve BaTiO
3one of effective measure of electronic component performance.
The method that tradition prepares tetragonal-phase barium titanate mainly adopts high temperature solid-state method, but the powder granule of preparation is thick, surfactivity is poor, reunion is serious, form segregation, and the size of particle and pattern also are difficult to control, and finally can greatly affect the electrical property of electronic devices and components.Hydrothermal method is a kind of evenly controlled material preparation method, has environmental protection, an advantage such as low, easy to control that consumes energy, and is commonly used to prepare the product of various multicomponent systems, also a kind of nano material preparation method commonly used, and this method is simple to operate, low for equipment requirements, with low cost.
Summary of the invention
The object of the present invention is to provide a kind of technique simply to prepare barium titanate BaTiO
3nanocrystalline method.
Barium titanate BaTiO of the present invention
3nanocrystalline preparation method comprises the following steps:
1) add deionized water, sequestrant and hydrolysis inhibitor in tetrabutyl titanate, stir 4-24 hour under normal pressure and 50-80 ℃, the pH value of controlling reactant is 2-3, obtain the water-soluble colloidal sol of titaniferous, the mol ratio of tetrabutyl titanate, deionized water, sequestrant and hydrolysis inhibitor is 1:150 ~ 300:0.1 ~ 0.6:0.01 ~ 0.04, described sequestrant is the one or both combination in quadrol and methyl ethyl diketone, and hydrolysis inhibitor is the one or both combination in hydrochloric acid and nitric acid.
2) take barium acetate by barium acetate and tetrabutyl titanate mol ratio 3:1 metering, barium acetate is added in deionized water, fully stir, form the aqueous solution of barium acetate;
3) potassium hydroxide being dissolved in to deionized water, by step 2) aqueous solution of the barium acetate that makes joins potassium hydroxide aqueous solution, then joins in the water-soluble colloidal sol of titaniferous of step 1), the suspension of the oxyhydroxide precipitation that obtains containing barium and titanium;
The suspension that 4) will contain the oxyhydroxide precipitation of barium and titanium is transferred in the reactor inner bag, reach the 70%-90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir at least 10 minutes, in reaction mass, the volumetric molar concentration of barium acetate is 0.375 mol/L, the volumetric molar concentration of tetrabutyl titanate is 0.125mol/L, and the volumetric molar concentration of potassium hydroxide is 2 ~ 4 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
5) the reactor inner bag that step 4) is disposed to reaction mass is placed in reactor, sealing, under 120 ℃-240 ℃, hydrothermal treatment consists is carried out in insulation in 6-24 hour, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain tetragonal-phase barium titanate BaTiO
3hollow is nanocrystalline.
In preparation process of the present invention, the reactor of use is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
In the present invention, the purity of said barium acetate, tetrabutyl titanate, potassium hydroxide, quadrol, methyl ethyl diketone and dehydrated alcohol all is not less than chemical pure.
The tetragonal-phase barium titanate BaTiO that the inventive method makes
3nanocrystalline size is 20-100 nm.
Beneficial effect of the present invention is:
The present invention adopts that simple solvent-thermal method has prepared that purity is high, good crystallinity, good dispersity, the narrow nanometer tetra phase barium titanate powder of size distribution.Technological process of the present invention is simple, and processing condition are easy to control, and cost is low, is easy to large-scale production.The cubic phase nano barium carbonate powder that the present invention makes is having broad application prospects in fields such as microelectronic device, high capacity capacitor, sensor, storage medium, piezoelectric ceramics, wave filters.
The accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the bismuth ferrite monocrystalline micron film for preparing of the present invention;
Fig. 2 is the stereoscan photograph of the bismuth ferrite monocrystalline micron film for preparing of the present invention;
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Example 1
1) add deionized water, quadrol and hydrochloric acid in tetrabutyl titanate, to be 1:260:0.3:0.03 stir 6 hours the mol ratio of tetrabutyl titanate, deionized water, quadrol and hydrochloric acid under normal pressure and 80 ℃, the pH value of controlling reactant is 2, obtains the water-soluble colloidal sol of titaniferous.
2) take barium acetate by barium acetate and tetrabutyl titanate mol ratio 3:1 metering, barium acetate is added in deionized water, fully stir, form the aqueous solution of barium acetate;
3) potassium hydroxide being dissolved in to deionized water, by step 2) aqueous solution of the barium acetate that makes joins potassium hydroxide aqueous solution, then joins in the water-soluble colloidal sol of titaniferous of step 1), the suspension of the oxyhydroxide precipitation that obtains containing barium and titanium;
The suspension that 4) will contain the oxyhydroxide precipitation of barium and titanium is transferred in the reactor inner bag, reach 90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 10 minutes, in reaction mass, the volumetric molar concentration of barium acetate is 0.375 mol/L, the volumetric molar concentration of tetrabutyl titanate is 0.125mol/L, and the volumetric molar concentration of potassium hydroxide is 4 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
5) the reactor inner bag that step 4) is disposed to reaction mass is placed in reactor, sealing, under 160 ℃, hydrothermal treatment consists is carried out in insulation in 12 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain tetragonal-phase barium titanate BaTiO
3hollow is nanocrystalline, and size is 20-100 nm.
Example 2
1) add deionized water, methyl ethyl diketone and nitric acid in tetrabutyl titanate, the mol ratio of tetrabutyl titanate, deionized water, methyl ethyl diketone and nitric acid is 1:280:0.37:0.04.Under normal pressure and 60 ℃, stir 10 hours, the pH value of controlling reactant is 3, obtains the water-soluble colloidal sol of titaniferous.
2) take barium acetate by barium acetate and tetrabutyl titanate mol ratio 3:1 metering, barium acetate is added in deionized water, fully stir, form the aqueous solution of barium acetate;
3) potassium hydroxide being dissolved in to deionized water, by step 2) aqueous solution of the barium acetate that makes joins potassium hydroxide aqueous solution, then joins in the water-soluble colloidal sol of titaniferous of step 1), the suspension of the oxyhydroxide precipitation that obtains containing barium and titanium;
The suspension of the oxyhydroxide that contains barium and the titanium precipitation that 4) will obtain is transferred in the reactor inner bag, reach 80% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 10 minutes, in reaction mass, the volumetric molar concentration of barium acetate is 0.375 mol/L, the volumetric molar concentration of tetrabutyl titanate is 0.125mol/L, and the volumetric molar concentration of potassium hydroxide is 4 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
5) the reactor inner bag that step 4) is disposed to reaction mass is placed in reactor, sealing, under 200 ℃, hydrothermal treatment consists is carried out in insulation in 6 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain tetragonal-phase barium titanate BaTiO
3hollow is nanocrystalline, and its XRD figure spectrum is shown in Fig. 1, as seen from the figure high, the good crystallinity of its purity; Fig. 2 is shown in by scanning electron microscope (SEM) photo.Tetragonal-phase barium titanate BaTiO
3the nanocrystalline size of hollow is 20-100 nm.
Example 3
1) add deionized water, methyl ethyl diketone and hydrochloric acid in tetrabutyl titanate, the mol ratio of tetrabutyl titanate, deionized water, methyl ethyl diketone and hydrochloric acid is 1:210:0.45:0.01.Under normal pressure and 50 ℃, stir 24 hours, the pH value of controlling reactant is 3, obtains the water-soluble colloidal sol of titaniferous.
2) take barium acetate by barium acetate and tetrabutyl titanate mol ratio 3:1 metering, barium acetate is added in deionized water, fully stir, form the aqueous solution of barium acetate;
3) potassium hydroxide being dissolved in to deionized water, by step 2) aqueous solution of the barium acetate that makes joins potassium hydroxide aqueous solution, then joins in the water-soluble colloidal sol of titaniferous of step 1), the suspension of the oxyhydroxide precipitation that obtains containing barium and titanium;
The suspension of the oxyhydroxide that contains barium and the titanium precipitation that 4) will obtain is transferred in the reactor inner bag, reach 70% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 10 minutes, in reaction mass, the volumetric molar concentration of barium acetate is 0.375 mol/L, the volumetric molar concentration of tetrabutyl titanate is 0.125mol/L, and the volumetric molar concentration of potassium hydroxide is 2mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
5) the reactor inner bag that step 4) is disposed to reaction mass is placed in reactor, sealing, under 120 ℃, hydrothermal treatment consists is carried out in insulation in 24 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain tetragonal-phase barium titanate BaTiO
3hollow is nanocrystalline, and size is 20-100 nm.
Claims (4)
1. a tetragonal-phase barium titanate BaTiO
3the preparation method that hollow is nanocrystalline is characterized in that comprising the following steps:
1) add deionized water, sequestrant and hydrolysis inhibitor in tetrabutyl titanate, stir 4-24 hour under normal pressure and 50-80 ℃, the pH value of controlling reactant is 2-3, obtain the water-soluble colloidal sol of titaniferous, the mol ratio of tetrabutyl titanate, deionized water, sequestrant and hydrolysis inhibitor is 1:150 ~ 300:0.1 ~ 0.6:0.01 ~ 0.04, described sequestrant is the one or both combination in quadrol and methyl ethyl diketone, and hydrolysis inhibitor is the one or both combination in hydrochloric acid and nitric acid;
2) take barium acetate by barium acetate and tetrabutyl titanate mol ratio 3:1 metering, barium acetate is added in deionized water, fully stir, form the aqueous solution of barium acetate;
3) potassium hydroxide being dissolved in to deionized water, by step 2) aqueous solution of the barium acetate that makes joins potassium hydroxide aqueous solution, then joins in the water-soluble colloidal sol of titaniferous of step 1), the suspension of the oxyhydroxide precipitation that obtains containing barium and titanium;
The suspension that 4) will contain the oxyhydroxide precipitation of barium and titanium is transferred in the reactor inner bag, reach the 70%-90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir at least 10 minutes, in reaction mass, the volumetric molar concentration of barium acetate is 0.375 mol/L, the volumetric molar concentration of tetrabutyl titanate is 0.125mol/L, and the volumetric molar concentration of potassium hydroxide is 2 ~ 4 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
5) the reactor inner bag that step 4) is disposed to reaction mass is placed in reactor, sealing, under 120 ℃-240 ℃, hydrothermal treatment consists is carried out in insulation in 6-24 hour, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain tetragonal-phase barium titanate BaTiO
3hollow is nanocrystalline.
2. tetragonal-phase barium titanate BaTiO according to claim 1
3the preparation method that hollow is nanocrystalline, is characterized in that reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
3. tetragonal-phase barium titanate BaTiO according to claim 1
3the preparation method that hollow is nanocrystalline, is characterized in that the purity of said barium acetate, tetrabutyl titanate, potassium hydroxide, quadrol, methyl ethyl diketone and dehydrated alcohol all is not less than chemical pure.
4. tetragonal-phase barium titanate BaTiO according to claim 1
3the preparation method that hollow is nanocrystalline, is characterized in that resulting tetragonal-phase barium titanate BaTiO
3the nanocrystalline size of hollow is 20-100 nm.
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| CN107151029B (en) * | 2017-04-28 | 2019-01-15 | 长安大学 | A kind of sol-gel self-combustion synthesis preparation process of tetra phase barium titanate powder |
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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 |
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