Preparation method of strontium titanate spherical nanocrystals

A nanocrystal, strontium titanate technology, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of complex preparation process, large grain size, large reaction particle size, etc., and meet the requirements of simple preparation operation. , Overcome the effect of high process complexity, large surface area and purity

Active Publication Date: 2019-06-07
XIDIAN UNIV
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Problems solved by technology

But at the same time, nano-strontium titanate also exhibits high surface energy, which is particularly prone to "agglomeration", which hinders its development and application.
For example: the high-temperature solid-phase preparation process requires very high energy, the reaction must be carried out at high temperature, the reaction particle size is large, the particle size distribution is wide, the solid mixing is difficult, the raw materials cannot be completely reacted, and the quality of the obtained powder is poor. The impurity content is high, and the chemical composition is not single; at the same time, because the particles are easy to agglomerate with the primary particles in the micron size range with a wide size distribution, it is difficult to meet the needs of some advanced electronic functional ceramic devices
Another example is the microwave synthesis method, whose reaction temperature is high, which tends to cause the grain size to be too large, which is easy to mix, and the powder with high purity cannot be obtained. The surface activity is poor, and it is easy to form agglomerates, and the reaction is not complete.
[0007] 2. The preparation process is complicated, the process is dangerous, and it is harmful to the environment. The results of the prepared samples need to be improved, and the preparation process cycle is too long.
The weak point of this method is: (1) the use of hydrothermal reaction kettle increases the danger and the complexity of preparation technology; , this washing waste liquid containing ethanol is harmful to the environment
The disadvantages of this method are: (1) the use of nitric acid and ammonia increases the danger and complexity of the preparation process; (2) the preparation process cycle is too long; (3) requires that a transparent gel must be prepared, and Vacuum drying is required, which increases the complexity of the preparation process
The disadvantages of this method are: (1) the strontium salt solution is added dropwise in the fatty alcohol solution of titanate / titanium alkoxide, which is unfavorable for industrialized large-scale production; (2) the gel must be Each of the four temperature ranges of 200-250°C, 300-450°C, 550-650°C, and 800-900°C must be sintered for 1-2 hours, and the gel must be aged until fat is precipitated on the surface. The preparation process requirements of alcohol solvent and water, so the preparation cycle time is too long, and the complexity of the preparation process is increased

Method used

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  • Preparation method of strontium titanate spherical nanocrystals
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Example 1: Preparation of strontium titanate nanocrystals with a spherical shape and a diameter of 0.1 μm.

[0053] Step 1, using butyl titanate and absolute ethanol to prepare a butyl titanate solution.

[0054] The configuration process of this step is as follows:

[0055] (1a) 250mL absolute ethanol is packed into a beaker;

[0056] (1b) With a needle tube, the density is 0.966g / cm 3 , a liquid butyl titanate with a volume of 8.8 mL;

[0057] (1c) Inject the butyl titanate extracted by the needle tube obtained in (1b) into 250mL of absolute ethanol, and at the same time mix and stir with an electric mechanical stirrer at a speed of 60 rpm for 2 minutes to obtain 0.10mol / L titanium butyl ester solution.

[0058] Step 2, using strontium nitrate and deionized water to prepare a strontium nitrate solution.

[0059] The configuration process of this step is as follows:

[0060] (2a) Dissolving 7.245g of strontium nitrate into 500mL of deionized water and mixing to p...

Embodiment 2

[0092] Example 2: Preparation of strontium titanate nanocrystals with a spherical shape and a diameter of 0.4 μm.

[0093] Step 1, using butyl titanate and absolute ethanol to prepare a butyl titanate solution.

[0094] First put 250mL of absolute ethanol into a beaker; then, use a needle to extract 3 , liquid butyl titanate with a volume of 30.8mL; after that, inject the butyl titanate extracted by the needle into 250mL of absolute ethanol, and at the same time mix and stir with an electric mechanical stirrer at a speed of 60 rpm for 2 minutes to obtain 0.35mol / L butyl titanate solution.

[0095] Step 2, using strontium nitrate and deionized water to prepare a strontium nitrate solution.

[0096] First, dissolve 17.45g of strontium nitrate into 500mL of deionized water and mix to prepare a strontium nitrate aqueous solution with a concentration of 0.165mol / L; then, place the funnel on the instrument support, put a clean beaker under the funnel, and place the filter paper F...

Embodiment 3

[0113] Example 3: Preparation of strontium titanate nanocrystals with a spherical shape and a diameter of 0.5 μm.

[0114] Step A, using butyl titanate and absolute ethanol to prepare a butyl titanate solution.

[0115] (A1) 250mL absolute ethanol is packed into a beaker;

[0116] (A2) With a needle tube, the density is 0.966g / cm 3 , a liquid butyl titanate with a volume of 42.3 mL;

[0117] (A3) Inject the butyl titanate extracted by the needle obtained in (A2) into 250 mL of absolute ethanol, and at the same time mix and stir for 2 minutes with an electric mechanical stirrer at a speed of 60 rpm to obtain 0.48 mol / L of titanium butyl ester solution.

[0118] Step B, using strontium nitrate and deionized water to prepare a strontium nitrate solution.

[0119] (B1) Dissolving 31.395g of strontium nitrate into 500mL of deionized water and mixing to prepare an aqueous strontium nitrate solution with a concentration of 0.297mol / L;

[0120] (B2) Put the funnel on the instrume...

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Abstract

The invention discloses a preparation method of strontium titanate spherical nanocrystals, and mainly solves the problems that the traditional preparation method of strontium titanate is complex, impurities are easy to generate, and the purity and the particle size of strontium titanate powder are difficult to meet the requirements. The method comprises the following steps: 1) adding an ampholyticsurfactant, dodecyl dimethyl amine ethyl lactone aqueous solution or a cocamidopropyl betaine aqueous solution, into a prepared strontium-titanium mixed solution to obtain an ampholytic surfactant modified strontium-titanium mixed solution; 2) adding a prepared sodium hydroxide solution into the strontium-titanium mixed solution to obtain an ampholytic surfactant modified strontium-titanium nanoprecipitate; 3) sequentially filtering, washing, drying, grinding, drying and sintering the nano precipitate to obtain the strontium titanate spherical nano crystal. The preparation method is simple in operation requirement, short in preparation period and suitable for industrial production. The product is good in dispersity and free of agglomeration, has the characteristics required by preparation of a grain boundary layer capacitor, and can be widely applied to circuits of a radio, a television and a computer.

Description

technical field [0001] The invention belongs to the technical field of chemical materials, and in particular relates to a method for preparing strontium titanate spherical nanocrystals, which can be used for photocatalysis, medium and high voltage large-capacity ceramic capacitors, grain boundary layer capacitors, piezoresistors, PTC thermistors, multiple Functional sensors, these electronic functional ceramic materials and devices, can also be used in the frontier development and research of micro-nano devices such as various microelectronic heterostructures, micro-sensors, solar cells, multilayer ceramic capacitors and micro-thermoelectric devices. Background technique [0002] Strontium titanate is a typical perovskite-type electronic material with unique chemical and physical properties, namely photocatalysis and piezoelectricity, ferroelectricity and high dielectric constant. Due to its excellent physical and chemical properties, Coupled with its excellent photocorrosio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00
Inventor 任庆利刘岩伟张茂林张志邈胡启航权曌
Owner XIDIAN UNIV
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