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Monodisperse high-purity lead iodide preparation method

A lead iodide, monodisperse technology, applied in the direction of lead halide, etc., can solve the problems of product quality failure, product phase impurity, etc., and achieve the effect of stable and reliable quality, high purity, and easy scale-up preparation

Active Publication Date: 2018-02-27
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Of course, the most important thing is the control of the synthetic process condition parameter range, which should be strictly guaranteed to be within the range of thermodynamically stable conditions for the formation of lead iodide, rather than the simultaneous appearance of other impurity lead-containing phases, which will lead to the final product Phase impurity will naturally directly lead to product quality failure

Method used

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  • Monodisperse high-purity lead iodide preparation method
  • Monodisperse high-purity lead iodide preparation method
  • Monodisperse high-purity lead iodide preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Prepare 10 liters of 0.1M lead nitrate solution and 10 liters of 0.11M potassium iodide solution, pre-adjust their respective pH to 3, and then add them dropwise to 10 liters of aqueous solution at a rate of 0.5 liters per minute (keep stirring , whose pH value is pre-adjusted to 3, and pre-prepared with 0.1% polyvinylpyrrolidone K-30 and 0.5% sodium citrate), after the dropwise addition, continue to stir and age for 10 hours, filter, use deionized Washed three times with water and dried at 80°C. The monodisperse lead iodide powder product can be obtained, and its typical morphology features are as follows figure 1 As shown, it is a flat, disc-shaped shape with a diameter of about 3 microns.

Embodiment 2

[0029] Prepare 10 liters of 0.25M lead chloride solution and 10 liters of 0.27M sodium iodide solution, pre-adjust their respective pH to 3.5, and then add them dropwise to 20 liters of aqueous solution at a rate of 1 liter / minute ( Keep stirring, the pH value is pre-adjusted to 3.5, and 0.5% concentration of polyvinylpyrrolidone K-30 is added in advance), after the dropwise addition, continue to keep stirring, age for 24 hours, filter, and wash with deionized water three times, Dry at 80°C. The monodisperse lead iodide powder product can be obtained, and its typical morphology features are as follows figure 1 As shown, it is a flat, disc-shaped shape with a diameter of about 3 microns.

Embodiment 3

[0031] Prepare 10 liters of 0.50M lead nitrate solution and 10 liters of 0.60M ammonium iodide solution, pre-adjust their respective pH to 2.5, and then add lead nitrate dropwise to the high-speed stirring potassium iodide solution at a speed of 1 liter / minute After the dropwise addition, continue to stir and age for 18 hours, filter, wash with deionized water three times, and dry at 80 degrees Celsius. A well-dispersed lead iodide powder product can be obtained, and its typical morphology features are as follows figure 2 As shown, it is a flat shape, with a width of hundreds of microns, and a small one of about 5 microns.

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Abstract

The invention relates to the technical field of monodisperse powdery material preparation and provides a monodisperse high-purity lead iodide preparation method. The preparation method comprises the steps of preparing a lead salt solution and a soluble iodate solution and adjusting a pH as 0.5 to 7; performing precipitation reaction on the lead salt solution and the soluble iodate solution in a contact mode to obtain precipitate turbid liquid of lead iodide; ageing for 1 to 48 hours at room temperature and filtering, washing and drying to obtain a high-purity lead iodide powder product. The preparation method disclosed by the invention has the beneficial effects of simpleness in operation, high purity, stable and reliable quality and easiness in expanding preparation in large scale.

Description

technical field [0001] The invention relates to the technical field of preparation of monodisperse powder materials, in particular to a method for preparing monodisperse high-purity lead iodide, and is especially suitable for the preparation and production of high-purity lead iodide materials as basic raw materials for making perovskite photovoltaic cells. Background technique [0002] Lead iodide is an important basic raw material for perovskite photovoltaic cells, and its chemical purity has a significant impact on the preparation quality and photoelectric conversion efficiency of subsequent battery thin film materials, so it should be strictly controlled during its preparation. [0003] The preparation method of lead iodide is varied, such as room temperature solid-phase chemical reaction method, but its purity and particle morphology and particle size and other aspects are difficult to guarantee; also have reverse microemulsion method to synthesize lead iodide nanorods, t...

Claims

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Application Information

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IPC IPC(8): C01G21/16
CPCC01G21/16C01P2004/03C01P2004/61C01P2006/80
Inventor 黄凯陈兴马瑞新王成彦
Owner UNIV OF SCI & TECH BEIJING
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