Method for preparing palladium and/or antimony-doping tin oxide nano-powder

A nano-powder, antimony-doped technology, applied in the direction of nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve the problems of unfavorable long-term large-scale production, affecting the final performance of powder, inconvenient storage and use, etc., to achieve the goal of preparation The effect of short cycle, low cost and mild conditions

Inactive Publication Date: 2010-09-08
NINGBO UNIV
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Problems solved by technology

[0005] 1) After the precursor is obtained by the co-precipitation method, the final product must be calcined. During the calcining process, impurities are easily introduced, resulting in the agglomeration of nano-powders and the segregation of doping elements, resulting in uneven doping and affecting Final properties of the powder
[0006] 2), using a large amount of concentrated hydrochloric acid, concentrated sulfuric acid, concentrated nitric acid or ammonia water as an

Method used

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  • Method for preparing palladium and/or antimony-doping tin oxide nano-powder

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Experimental program
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Effect test

specific Embodiment 1

[0030] Step 1, 2.7078g of SnCl 2 2H 2 O was dissolved in 20mL of ethanol and stirred to form a 0.6mol / L transparent solution; according to Pd 2+ with Sn 2+ The molar ratio is 2.5%, weigh an appropriate amount of PdCl 2 Dissolve in 1.0mol / L hydrochloric acid aqueous solution, and stir to form a 0.3mol / L solution; Dissolve NaOH in a certain amount of deionized water, and stir to form a 1mol / L NaOH solution;

[0031] Step 2, under stirring conditions, the PdCl configured in step 1 2 The solution was evenly added dropwise to the SnCl 2solution, and then stirred for 10 minutes to form a mixed solution;

[0032] Step 3, while stirring, NaOH solution is evenly added dropwise to the mixed solution obtained in Step 2 until the pH value is 12, and then stirred for 1 hour to form a precursor suspension with a large amount of precipitation;

[0033] Step 4, transfer the precursor suspension obtained in step 3 to an autoclave, react at 180° C. for 12 hours, and then naturally cool to...

specific Embodiment 2

[0036] Step 1, 2.7078g of SnCl 2 2H 2 O was dissolved in 20mL of ethanol and stirred to form a 0.6mol / L transparent solution; according to Sb 3+ with Sn 2+ The molar ratio is 2.5%, weigh an appropriate amount of SbCl 3 Dissolve in water and form a 0.3mol / L suspension with white precipitate after stirring; Dissolve NaOH in a certain amount of deionized water and form a 1mol / L NaOH solution after stirring;

[0037] Step 2, under stirring conditions, the SbCl configured in step 1 3 The suspension was evenly added dropwise to the SnCl 2 solution, and then stirred for 20 minutes to form a mixed solution;

[0038] Step 3, while stirring, NaOH solution is evenly added dropwise to the mixed solution described in step 2 until the pH value is 12, and then stirred for 1 hour to form a precursor suspension accompanied by a large amount of precipitation;

[0039] Step 4, transferring the precursor suspension described in step 3 to a high-pressure reactor, reacting at 180° C. for 24 h...

specific Embodiment 3

[0042] Step 1, 2.7078g of SnCl 2 2H 2 O was dissolved in 20mL of ethanol and stirred to form a 0.6mol / L transparent solution; according to Pd 2+ with Sn 2+ The molar ratio is 2.5%, weigh an appropriate amount of PdCl 2 Dissolve in 1.0mol / L hydrochloric acid aqueous solution, and form a 0.3mol / L purplish red solution after stirring; according to Sb 3+ with Sn 2+ The molar ratio is 2.5%, weigh an appropriate amount of SbCl 3 Dissolve in water and form a 0.3mol / L suspension with white precipitate after stirring; Dissolve NaOH in a certain amount of deionized water and form a 1mol / L NaOH solution after stirring;

[0043] Step 2, under agitation conditions, the PdCl configured in step 1 is respectively 2 and SbCl 3 The solution was evenly added dropwise to the SnCl 2 solution, and then stirred for 30 minutes to form a mixed solution;

[0044] Step 3, while stirring, NaOH solution is evenly added dropwise to the mixed solution described in step 2 until the pH value is 12, a...

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Abstract

The invention discloses a method for preparing palladium and/or antimony-doping tin oxide nano-powder. The method mainly comprises the following steps of: mixing raw materials according to the molar doping ratio of Pd<2+> and/or Sb<3+> to Sn<2+> of 0.5 to 3.5 and dropwise adding at least one of the solution of PdCl2 and the suspension of SbCl3 into the solution of tin salt with stirring to form mixed solution, wherein the raw materials comprise 0.2 to 1 mol/L solution of tin salt, 0.1 to 0.5 mol/L solution of palladium chloride (PbCl2), 0.1 to 0.5 mol/L suspension of antimony chloride (SbCl3)and 0.4 to 1 mol/L solution of alkali source; adding the solution of alkali source dropwise into the mixed solution with stirring until the pH value is between 9 and 13; stirring the solution to formprecursor suspension with a large amount of precipitate; transferring the precursor suspension to a high-pressure reactor to perform reaction for 12 to 36 hours at the temperature of between 100 and 200 DEG C and naturally cooling to room temperature to obtain a hydrothermal product; washing the hydrothermal product for multiple times by using deionized water and ethanol and detecting the productby using silver nitrate until the Cl<-> is removed completely; and drying at the temperature of between 70 and 100 DEG C to obtain the palladium and/or antimony-doping tin oxide nano-powder. The method has the advantages of simple process, environmental friendliness and suitability for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of tin oxide nano powder, in particular to a preparation method of palladium and / or antimony doped tin oxide nano powder. Background technique [0002] SnO 2 With excellent photoelectric characteristics and sensitivity to reducing gases, it has been widely used in the fields of gas sensor materials, transparent conductive powders and photocatalytic materials. When SnO 2 After the grain size of the material enters the nanoscale, it shows many special physical and chemical properties due to the unique small size effect, quantum size effect and surface effect of nanomaterials, so that SnO 2 Nanoparticles have shown great advantages in applications such as gas sensing, transparent conduction, and photocatalysis. But due to SnO 2 Nanoparticles have a high specific surface energy and belong to a thermodynamically unstable system. In order to achieve a stable state, the particles will spontaneously agglomerate...

Claims

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Application Information

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IPC IPC(8): B82B3/00
Inventor 谭瑞琴郭艳群李月杨晔宋伟杰徐铁锋聂秋华
Owner NINGBO UNIV
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