Method for preparing ball-flower-shaped gamma-bismuth trioxide powder

A bismuth oxide, spherical technology, applied in chemical instruments and methods, inorganic chemistry, bismuth compounds, etc., can solve problems such as weak relative strength, achieve uniform morphology, low synthesis temperature, and good repeatability.

Inactive Publication Date: 2012-06-13
临沂润泰新型建材有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, Bi(OH) with relatively weak intensity exists in the spectra of both samples 3 Crystal diffraction peaks, indicating that in the high temperature and high pressure environment of the hydrothermal synthesis system, there are still some Bi(OH) 3 Not fully reacted

Method used

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  • Method for preparing ball-flower-shaped gamma-bismuth trioxide powder
  • Method for preparing ball-flower-shaped gamma-bismuth trioxide powder
  • Method for preparing ball-flower-shaped gamma-bismuth trioxide powder

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Embodiment 1）

[0036] This embodiment prepares flower spherical γ-Bi 2 o 3 The powder method includes the following steps:

[0037] ① Configuration of bismuth salt solution: 16.9596g (0.035mol) of bismuth nitrate pentahydrate (Bi(NO 3 ) 3 ·5H 2 O) added to 60ml of ethylene glycol, stirred to dissolve it to obtain a bismuth salt solution, Bi in the resulting solution 3+ The concentration is 0.58mol / L.

[0038] ②Configuration of reaction solution: Mix 60mL of sodium hydroxide solution with a concentration of 3mol / L, 180mL of water and 1.5606g (0.00078mL) polyethylene glycol 2000 (hereinafter referred to as PEG-2000, analytically pure, chemical reagent of Sinopharm Group) under stirring Co., Ltd., the same below) were sequentially added to the bismuth salt solution prepared in step ①, and continued to stir for 60 minutes to obtain a reaction solution.

[0039] ③ Hydrothermal reaction: Add the reaction solution prepared in step ② into a hydrothermal reaction kettle with a polytetrafluoroet...

Embodiment 2）

[0047] This embodiment prepares flower spherical γ-Bi 2 o 3 The rest of the powder method is the same as in Example 1, except that in step ③, the time for the reaction solution to undergo hydrothermal reaction at 200° C. is 4 hours.

[0048] The X-ray powder diffraction pattern of the product is shown in image 3 , there are characteristic diffraction peaks at 2θ=27.40°, 32.55° and 51.95°, which is the same as that of γ-Bi in JCPDF card (card number 45-1344) 2 o 3 The characteristic diffraction peaks at 2θ=24.40°, 30.10°, 41.21°, 43.17°, 45.10°, 55.18° and 61.26° also correspond to the above-mentioned standard spectrum, indicating that the obtained product is mainly cubic structure γ -Bi 2 o 3 ; In addition, the impurity crystal diffraction peaks on the XRD diffraction pattern are weak, indicating that the prepared γ-Bi 2 o 3 The crystal phase purity is high.

[0049] The SEM photo of the product is shown in Figure 4 , The SEM photo of the powder shows that the parti...

Embodiment 3）

[0052] This embodiment prepares flower spherical γ-Bi 2 o 3 The rest of the powder method is the same as in Example 1, except that in step ③, the time for the reaction solution to undergo hydrothermal reaction at 200° C. is 18 hours.

[0053] The X-ray powder diffraction pattern of the product is shown in Figure 5 , with γ-Bi in the JCPDF card (card number 45-1344) 2 o 3 The diffraction peaks are consistent, indicating that the obtained product is mainly cubic structure γ-Bi 2 o 3 ; In addition, the impurity crystal diffraction peaks on the XRD diffraction pattern are weak, indicating that the prepared γ-Bi 2 o 3 The crystal phase purity is high.

[0054] The SEM photo of the product is shown in Image 6 , The SEM photo of the powder shows that the particles are flower-shaped, with a large specific surface area and a particle size of 1.5-5 μm, which is greatly reduced compared with Example 1, indicating that the particle size is gradually reduced with the prolongation...

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Abstract

The invention discloses a method for preparing ball-flower-shaped gamma-bismuth trioxide powder, which comprises the following steps: 1 adding Bi(NO3)3 5H2O into glycol, and performing stirring to enable the Bi(NO3)3 5H2O to be dissolved, 2 sequentially adding NaOH solution, water and polyethylene glycol into prepared bismuth salt solution during the stirring to obtain reaction solution, adding the prepared reaction solution into a hydrothermal reaction kettle containing a polytetrafluoroethylene substrate, and performing hydrothermal reaction for producing Bi2O3 in an airtight state, and 3 cooling an obtained material to the room temperature and then performing air pump filtration, washing and drying to obtain a gamma-Bi2O3 powder product. The prepared gamma-Bi2O3 has uniform morphology and good dispersity. The microstructure is in a ball-like shape, and further, the ball-like shape is a ball-flower shape with diameter of 1-25 micrometers and large specific surface area. The thickness of nanometer sheets for forming micro-balls is smaller than 100 micrometers, visible light response is good, and photo-catalytic activity is high.

Description

technical field [0001] The invention relates to the field of oxide powder preparation, in particular to a flower spherical γ-Bi 2 o 3 Method of powder preparation. Background technique [0002] Bismuth oxide belongs to P-type semiconductor and is an advanced semiconductor functional material, which is widely used in industries such as electronic ceramics, optoelectronic devices and glazes. It is generally believed that bismuth oxide has four crystal forms of α, β, γ and δ. where α-Bi 2 o 3 and δ-Bi 2 o 3 is a thermodynamically stable crystal form, α-Bi 2 o 3 It exists stably below 730°C in a monoclinic structure, and δ-Bi with a cubic fluorite structure 2 o 3 It exists stably in the range of 730°C to 825°C; at 650°C, β-Bi with tetragonal structure will also appear 2 o 3 and body-centered cubic structure γ-Bi 2 o 3 metastable compounds. γ-Bi 2 o 3 It is an optically active cubic crystal with very high oxygen ion conductivity and can be used as an electrolyte ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G29/00B82Y40/00
Inventor 张春勇关明云舒莉文颖频朱炳龙郑纯智单万建张继振
Owner 临沂润泰新型建材有限公司
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