Preparation method for necklace shaped lead titanate nano wire

A lead titanate and nanowire technology, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of difficult to control the production process, uneven particle size distribution, and low production efficiency.

Inactive Publication Date: 2009-02-18
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional preparation method of lead titanate powder is a high-temperature solid-phase method, which is to combine PbO and TiO 2 It is prepared by burning at high temperature after mixing. Since the reaction is between solid phase and solid phase and is completed at high temperature, the reaction is uneven, the reactivity is poor, the product has large particle size and low purity.
In order to overcome the shortcomings of the solid-phase method, wet chemical preparation methods have received more and more attention, including chemical co-precipitation, hydrothermal, sol-gel methods, etc., but these methods still have some shortcomings: the chemical co-precipitation method p...

Method used

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  • Preparation method for necklace shaped lead titanate nano wire
  • Preparation method for necklace shaped lead titanate nano wire
  • Preparation method for necklace shaped lead titanate nano wire

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Accurately weigh 11.09g of H 2 C 2 o 4 2H 2 O is dissolved in deionized water (dubbed into H 2 C 2 o 4 The concentration is 0.88mol / L), add 13.60mL of butyl titanate (the amount of oxalic acid is 2.2 times that of butyl titanate), stir until the solution is clear, transfer it to a 100mL volumetric flask, and adjust the pH value with ammonia water is 3, dilute to the mark with deionized water, and prepare [TiO(C 2 o 4 ) 2 ] 2- solution.

[0028] (2) Take 22mL cyclohexane, 1.13mL octylphenol polyoxyethylene (9) ether (Triton X-100), 1.07mL n-hexanol and 1mL0.42mol / L Pb(NO 3 ) 2 solution (ω 0 =30, P=4.6) into a container, after the components are fully mixed, stir vigorously on a magnetic stirrer for 20 minutes to prepare a uniform and clear Pb-containing 2+ of microemulsions. 1mL 0.42mol / L of Pb(NO 3 ) 2 The solution was changed to 1mL of 0.40mol / L [TiO(C 2 o 4 ) 2 ] 2- Solution, the same amount of other reagents, prepared in the same way containin...

Embodiment 2

[0031] (1) Accurately weigh 19.66g of H 2 C 2 o 4 2H 2 O is dissolved in deionized water (dubbed into H 2 C 2 o 4 The concentration is 1.56mol / L), add 17.06mL propyl titanate (the amount of oxalic acid is 2.6 times that of propyl titanate), stir until the solution is clear, transfer it to a 100mL volumetric flask, adjust the pH value with ammonia water to about is 2.5, dilute to the mark with deionized water, and prepare [TiO(C 2 o 4 ) 2 ] 2- solution.

[0032] (2) Take 23mL isooctane, 1.26mL alkylphenol polyoxyethylene (10) ether (OP-10), 1.03mL n-octanol and 1mL 0.66mol / L PbAc 2 solution (ω 0 =28, P=4.0) into a container, after the components are fully mixed, stir vigorously on a magnetic stirrer for 10 minutes to prepare a uniform and clear Pb-containing 2+ of microemulsions. 1mL of 0.66mol / L PbAc 2 The solution was changed to 1mL of 0.60mol / L [TiO(C 2 o 4 ) 2 ] 2- Solution, the same amount of other reagents, prepared in the same way containing [TiO(C 2 o...

Embodiment 3

[0035] (1) Accurately weigh 24.71g H 2 C 2 o 4 2H 2 O is dissolved in deionized water (dubbed into H 2 C 2 o 4 The concentration is 1.96mol / L), add 7.69mL titanium tetrachloride (the amount of oxalic acid is 2.8 times that of titanium tetrachloride), stir until the solution is clear, then transfer to a 100mL volumetric flask, adjust the pH value with ammonia water to about is 2.3, dilute to the mark with deionized water, and prepare [TiO(C 2 o 4 ) 2 ] 2- solution.

[0036] (2) Take 21mL of heptane, 1.06mL of octylphenol polyoxyethylene (9) ether (Triton X-100), 1.06mL of n-pentanol and 1mL of 0.71mol / L Pb(NO 3 ) 2 solution (ω 0 =32, P=5.0) into a container, after the components are fully mixed, stir vigorously on a magnetic stirrer for 30 minutes to prepare a uniform and clear Pb-containing 2+of microemulsions. 1mL0.71mol / L of Pb(NO 3 ) 2 The solution was changed to 1 mL of 0.70 mol / L [TiO(C 2 o 4 ) 2 ] 2- Solution, the same amount of other reagents, prepar...

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Abstract

The invention provides a method for preparing the necklace-shaped lead titanate nano-wire, which comprises the following steps: firstly after the titanic acid ester or soluble titanium salt is reacted with oxalic acid solution to form the complex ion [TiO(C2O4)2]<2->, surface active agent, cosurfactant and fat phase are used to be mixed with the soluble lead salt solution and the [TiO(C2O4)2]<2-> solution to respectively form two uniform and transparent microemulsions containing Pb<2+> and TiO(C2O4)2]<2->; two microemulsions are mixed and reacted, and then are aged, centrifuged and separated, and washed, dried and calcined to get the necklace-shaped lead titanate nano-wire with the length about 450 nm to 2200 nm, and the wider diameter about 60 to 145 nm and the narrower diameter about 40 to 115 nm. The method can conveniently control the size and the shape of the particles of the product, and has the advantages of simple production craftwork, safe production process, uneasy reunion and damage of the particles of the product, high purity of the product, high production efficiency and low implementation cost, and can be widely used for preparing the nano materials with different shapes.

Description

technical field [0001] The invention relates to a method for preparing inorganic functional nanometer materials, in particular to a method for preparing necklace-like lead titanate nanowires by adopting an inverse microemulsion method. Background technique [0002] Lead titanate (PbTiO 3 ) is a ferroelectric material with a perovskite structure, because it has the advantages of high Curie temperature (greater than 490 ° C), small dielectric constant and large pyroelectric coefficient, as well as excellent pyroelectric, piezoelectric, Ferroelectric, electro-optic and other properties have been generally valued by people. It is an important material for making high-frequency filters, infrared detectors, ultrasonic transducers and electro-optic devices. The traditional preparation method of lead titanate powder is a high-temperature solid-phase method, which is to combine PbO and TiO 2 It is prepared by high-temperature combustion after mixing. Since the reaction is between ...

Claims

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Application Information

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IPC IPC(8): C01G23/00
Inventor 朱启安张超龚敏雍高兵项尚
Owner XIANGTAN UNIV
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