Low-temperature direct-precipitation preparation method of sub-micron grade strontium titanate

A sub-micron strontium titanate technology, applied in the direction of titanate, alkaline earth metal titanate, chemical instruments and methods, can solve the problems of hard agglomeration and increase the cost of exhaust gas recovery, and achieve fine and uniform particle size, low cost Low cost and convenient effect

Inactive Publication Date: 2016-05-04
JIANGNAN UNIV
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Problems solved by technology

The literature "Zhu Qi'an, Shi Rongkai, Huang Boqing, Tan Yiwen. Research on a new method for the synthesis of strontium titanate powder [J]. Inorganic Salt Industry, 2002, 34(1): 5-7" uses titanium tetrachloride and strontium chloride as raw materials, Strontium titanate powder with high purity, uniform size distribution and small particle size (average particle size <500nm) was prepared by chemical co-precipitation method with ammonium carbonate and ammonia water as precipitant, but this method needs to be calcined at a high temperature of 880°C. The ammonium carbonate and ammonia water used will produce nitrogen-containing toxic gases during the calcination process, which will not only increase the cost of waste gas recovery in actual industrial production, but also easily cause hard agglomeration during high-temperature calcination

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  • Low-temperature direct-precipitation preparation method of sub-micron grade strontium titanate
  • Low-temperature direct-precipitation preparation method of sub-micron grade strontium titanate
  • Low-temperature direct-precipitation preparation method of sub-micron grade strontium titanate

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Embodiment 1

[0021] Measure the prepared 1.2mol / L SrCl with a graduated cylinder 2 solution (19.8mL) and 1.2mol / L of TiCl 4 solution (18mL), that is, the molar ratio of strontium ions and titanium ions is 1.1: 1 and stirred and mixed evenly, then PEG4000 is added to the system as a dispersant (wherein the amount of PEG4000 added is SrTiO 3 0.5% of theoretical output) fully stirred; Add 6mol / L NaOH solution 22mL in above-mentioned mixed solution, guarantee that the pH=13 of suspension liquid after reaction finishes; The feed liquid that will mix is ​​added to be placed in the constant temperature water bath In the three-necked flask, one of the side ports on both sides of the three-necked flask is equipped with a thermometer sleeve and a thermometer, and the other is equipped with a serpentine reflux condenser. Use an electric mixer as the stirring device, adjust the speed of the electric mixer to 250r / min, and raise the temperature to 50°C. Time starts counting, and after 4 hours, turn of...

Embodiment 2

[0026] Carry out according to the method in embodiment 1, reaction temperature is 75 ℃, and difference is that dispersant adopts PEG2000 (wherein the addition of PEG2000 is SrTiO 3 0.5% of theoretical yield).

[0027] image 3 It is the SEM of the product obtained in Example 2. It can be seen from the figure that when the strontium titanate powder is prepared by the low-temperature direct precipitation method, adding PEG2000 as a dispersant can improve the agglomeration of the powder, but the effect is not as good as that of PEG4000, and the shape is a regular spherical shape. , the distribution and size are uniform, the shape is cubic phase, the particle size of the powder is small, most of them are around 60nm, which is similar to the XRD calculation result, and the particle size has reached the nanometer level.

Embodiment 3

[0029] The raw strontium chloride solution was made from SrCO 3 (AR) and hydrochloric acid solution reaction system. Accurately weigh 3.51gSrCO 3 , the weighed SrCO 3 Put it into the beaker; then slowly add the dilute hydrochloric acid solution into the beaker until no more bubbles are generated; use a graduated cylinder to measure the prepared 1.2mol / L TiCl 4 solution (18mL), that is, the molar ratio of strontium ion and titanium ion is 1.1: 1, stir and mix evenly, fully stir; add 22mL of 6mol / L NaOH solution to the above mixed solution to ensure that the pH of the suspension after the reaction is finished=13 ; Add the mixed material liquid into the three-necked flask placed in the constant temperature water bath, use the electric mixer as the stirring device, adjust the speed of the electric mixer to 250r / min, start timing when the temperature rises to 75°C, and turn off the constant temperature water bath after 4h and an electric mixer, stand still for 0.5h, and carry ou...

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Abstract

The invention provides a low-temperature direct-precipitation preparation method of sub-micron grade strontium titanate, and belongs to the technical field of superfine powder material preparation. The method comprises the following steps: adding a dispersing agent into a three-neck flask which is filled with strontium oxide and titanium oxychloride mixed solution, and uniformly stirring; dropwise adding a sodium hydroxide solution; heating and stirring to react for a period; and filtering, washing and drying the precipitated substance to obtain the strontium titanate with excellent dispersion. The preparation method does not need high temperature calcining, has small environmental pollution and simple process, does not need specific equipment, and is convenient for industrial production; and the prepared strontium titanate powder has uniform grain diameter which is about 60nm, high purity and good dispersion.

Description

technical field [0001] The invention relates to a preparation method of a functional powder material, which belongs to the technical field of ultrafine powder material preparation. Background technique [0002] Strontium titanate powder material is an important electronic ceramic material in the industry. It has the advantages of heat sensitivity, superconductivity, semiconductivity, good dielectric properties, low power loss, and good temperature stability. Therefore, it is widely used in the manufacture of electronic components such as thermistors, high voltage capacitors, interlayer capacitors and multifunctional sensors. In order to meet the higher material property requirements of electronic components in the future, it is necessary to prepare strontium titanate powder materials with fine and uniform particle size and good dispersibility. [0003] Generally speaking, there are four methods for preparing strontium titanate: high-temperature solid phase sintering method;...

Claims

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Application Information

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IPC IPC(8): C01G23/00
CPCC01G23/006C01P2002/72C01P2002/82C01P2004/03C01P2004/64
Inventor 商少明刘欢欢顾丹陈秀英许虎君高海燕沈洁
Owner JIANGNAN UNIV
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