CN106379938A - Method for preparing black alpha-Bi2O3 powder material - Google Patents

Method for preparing black alpha-Bi2O3 powder material Download PDF

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Publication number
CN106379938A
CN106379938A CN201610813287.9A CN201610813287A CN106379938A CN 106379938 A CN106379938 A CN 106379938A CN 201610813287 A CN201610813287 A CN 201610813287A CN 106379938 A CN106379938 A CN 106379938A
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dusty material
black
yellow
alpha
powder material
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CN201610813287.9A
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CN106379938B (en
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尚军
陈秋艳
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Henan Normal University
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Henan Normal University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a method for preparing a black alpha-Bi2O3 powder material and belongs to the technical field of synthesis of photoelectric materials. According to the key points of the technical scheme of the invention, the method comprises the following steps: maintaining the temperature of bismuth nitrate pentahydrate in a muffle furnace to be 500 DEG C for 6 hours, naturally cooling, grinding, thereby obtaining a yellow alpha-Bi2O3 powder material; adding the obtained yellow alpha-Bi2O3 powder material into a reaction container, adding deionized water and hydrogen peroxide, irradiating by using a mercury lamp with the power of 300W under the magnetic stirring condition for an hour, standing, pouring the supernatant liquor, and drying the precipitate in a drying oven, thereby obtaining the target product, namely the black alpha-Bi2O3 powder material. According to the method disclosed by the invention, the preparation process is simple and feasible, the synthesis period is short, and the prepared black alpha-Bi2O3 powder material has the absorption edge of 1902nm, has the optical wave utilization rate higher than that of the yellow alpha-Bi2O3 material, and has potential application values in the photoelectric material aspect.

Description

One kind prepares black α-Bi2O3The method of dusty material
Technical field
The invention belongs to the synthesis technical field of photoelectric material is and in particular to one kind prepares black α-Bi2O3Dusty material Method.
Background technology
China's bismuth aboundresources, in recent years, more than 6000 ton, application is quite varied for annual production.Bi2O3As bismuth depth of origin A kind of product after processing, is a kind of advanced functional material, ceramic material [J. Alloys Compd., 2014, pp627- 632], electrolyte [Ceram. Int., 2016, pp16262-16265], ferroelectric material [J.Eur.Ceram.Soc., 2014, pp102-108], the side such as catalysis material [Ceram. Int., 2016, pp2013-2020], photoelectric material and sensor There is important application in face, and increasing people begins to focus on α-Bi2O3.It has been reported that α-Bi2O3ABSORPTION EDGE be 450- 470nm, appearance color is yellow, the utilization rate extremely low [Mater. Lett., 2011, pp988-990] to light wave.Therefore, have A kind of α-Bi that can effectively improve light wave utilization rate of necessary design2O3The novel synthesis of material.
Content of the invention
Present invention solves the technical problem that there is provided that a kind of synthesis technique is simple, the cycle is shorter prepares black α-Bi2O3 The method of dusty material.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, one kind prepares black α-Bi2O3Dusty material Method is it is characterised in that concretely comprise the following steps：
（1）Yellow α-Bi2O3The synthesis of dusty material, five water bismuth nitrate is placed in Muffle furnace and is incubated 6 hours in 500 DEG C, from Grind after so cooling down and obtain yellow α-Bi2O3Dusty material；
（2）Black α-Bi2O3The synthesis of dusty material, by step（1）Yellow α-the Bi obtaining2O3Dusty material is placed in reaction to be held In device, add deionized water and hydrogen peroxide, the Hg lamp irradiation being 300W with power under conditions of magnetic agitation 1 hour, standing After outwell supernatant, precipitation is placed in drying baker and is dried to obtain target product black α-Bi2O3Dusty material.
Further preferably, step（2）The addition of middle hydrogen peroxide and yellow α-Bi2O3The mass ratio of dusty material is 2.5- 6:0.35-0.5.
Further preferably, step（2）In drying condition be that temperature less than 100 DEG C is dried more than 2 hours.
Preparation process simple possible of the present invention, synthesis cycle is shorter, prepared black α-Bi2O3The ABSORPTION EDGE of dusty material For 1902nm, it is much larger than yellow α-Bi to the utilization rate of light wave2O3Material, has potential using value in terms of photoelectric material.
Brief description
Fig. 1 is the yellow α-Bi that the embodiment of the present invention 1 is obtained2O3Dusty material and black α-Bi2O3The powder of dusty material Abosrption spectrogram；
Fig. 2 is the yellow α-Bi that the embodiment of the present invention 1 is obtained2O3Dusty material and black α-Bi2O3The X-ray of dusty material is spread out Penetrate collection of illustrative plates；
Fig. 3 is the yellow α-Bi that the embodiment of the present invention 1 is obtained2O3The scanning electron microscope (SEM) photograph of dusty material；
Fig. 4 is the black α-Bi that the embodiment of the present invention 1 is obtained2O3The scanning electron microscope (SEM) photograph of dusty material.
Specific embodiment
By the following examples the above of the present invention is described in further details, but this should not be interpreted as this The scope inventing above-mentioned theme is only limitted to below example, all belongs to this based on the technology that the above of the present invention is realized Bright scope.
Embodiment 1
（1）Yellow α-Bi2O3The synthesis of dusty material
1g five water bismuth nitrate is placed in Muffle furnace and is incubated 6 hours in 500 DEG C, grind after natural cooling and obtain yellow α-Bi2O3 Dusty material；
（2）Black α-Bi2O3The synthesis of dusty material
By 0.04g step（1）Yellow α-the Bi obtaining2O3Dusty material is placed in reaction vessel, add 100mL deionized water and The Hg lamp irradiation that 0.4g hydrogen peroxide is 300W with power under conditions of magnetic agitation 1 hour, outwells supernatant after standing, Precipitation is placed in drying baker and obtains within 150 minutes target product black α-Bi in 80 DEG C of dryings2O3Dusty material.
Embodiment 2
（1）Yellow α-Bi2O3The synthesis of dusty material
1g five water bismuth nitrate is placed in Muffle furnace and is incubated 6 hours in 500 DEG C, grind after natural cooling and obtain yellow α-Bi2O3 Dusty material；
（2）Black α-Bi2O3The synthesis of dusty material
By 0.2g step（1）Yellow α-the Bi obtaining2O3Dusty material is placed in reaction vessel, add 100mL deionized water and The Hg lamp irradiation that 1g hydrogen peroxide is 300W with power under conditions of magnetic agitation 1 hour, outwells supernatant after standing, sinks Shallow lake is placed in drying baker and obtains within 180 minutes target product black α-Bi in 70 DEG C of dryings2O3Dusty material.
Embodiment 3
（1）Yellow α-Bi2O3The synthesis of dusty material
1g five water bismuth nitrate is placed in Muffle furnace and is incubated 6 hours in 500 DEG C, grind after natural cooling and obtain yellow α-Bi2O3 Dusty material；
（2）Black α-Bi2O3The synthesis of dusty material
By 0.04g step（1）Yellow α-the Bi obtaining2O3Dusty material is placed in reaction vessel, adds deionized water and 0.68g The Hg lamp irradiation that hydrogen peroxide is 300W with power under conditions of magnetic agitation 1 hour, outwells supernatant after standing, precipitation It is placed in drying baker and obtain within 120 minutes target product black α-Bi in 100 DEG C of dryings2O3Dusty material.
The present invention adopts new preparation technology, in yellow α-Bi2O3Add hydrogen peroxide in dusty material and deionized water, In the presence of hydrogen peroxide, mercury lamp During Illumination produces Lacking oxygen, powder is changed into black from yellow, finally gives black α-Bi2O3.Prepare black α-Bi with the method2O3Dusty material process is easy, and cost of material is cheap, and being suitable to large-scale production makes With.
Embodiment above describes ultimate principle, principal character and the advantage of the present invention, the technical staff of the industry should Understand, the present invention is not restricted to the described embodiments, the simply explanation present invention's described in above-described embodiment and description is former Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within In the scope of protection of the invention.

Claims (3)

1. one kind prepares black α-Bi2O3The method of dusty material is it is characterised in that concretely comprise the following steps：
（1）Yellow α-Bi2O3The synthesis of dusty material, five water bismuth nitrate is placed in Muffle furnace and is incubated 6 hours in 500 DEG C, natural Grind after cooling and obtain yellow α-Bi2O3Dusty material；
（2）Black α-Bi2O3The synthesis of dusty material, by step（1）Yellow α-the Bi obtaining2O3Dusty material is placed in reaction vessel In, add deionized water and hydrogen peroxide, the Hg lamp irradiation being 300W with power under conditions of magnetic agitation 1 hour, after standing Outwell supernatant, precipitation is placed in drying baker and is dried to obtain target product black α-Bi2O3Dusty material.
2. according to claim 1 prepare black α-Bi2O3The method of dusty material it is characterised in that：Step（2）In double The addition of oxygen water and yellow α-Bi2O3The mass ratio of dusty material is 2.5-6:0.35-0.5.
3. according to claim 1 prepare black α-Bi2O3The method of dusty material it is characterised in that：Step（2）In Drying condition is that the temperature less than 100 DEG C is dried more than 2 hours.
CN201610813287.9A 2016-09-10 2016-09-10 One kind prepares black α Bi2O3The method of dusty material Expired - Fee Related CN106379938B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107416899A (en) * 2017-04-05 2017-12-01 河南师范大学 A kind of nano wire α Bi2O3The preparation method of dusty material
CN107899602A (en) * 2017-11-01 2018-04-13 河南师范大学 A kind of preparation method with visible light-responded grey basic bismuth nitrate catalysis material
CN108927137A (en) * 2018-07-20 2018-12-04 河南师范大学 A kind of preparation method of carbon doping bismuth oxide catalysis material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787355A (en) * 2012-09-07 2012-11-21 江西理工大学 Method for preparing alpha-Bi2O3 monocrystalline micron rods
CN103253704A (en) * 2013-04-12 2013-08-21 武汉理工大学 Semiconductor porous bismuth oxide nanosphere and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102787355A (en) * 2012-09-07 2012-11-21 江西理工大学 Method for preparing alpha-Bi2O3 monocrystalline micron rods
CN103253704A (en) * 2013-04-12 2013-08-21 武汉理工大学 Semiconductor porous bismuth oxide nanosphere and preparation method and application thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
A. J. SALAZAR-PÉREZ等: "Structural evolution of Bi2O3 prepared by thermal oxidation of bismuth nano-particles", 《SUPERFICIES Y VACÍO》 *
DENG HONG-YAN等: "A Transition Phase in the Transformation from 𝛼-, 𝛽- and 𝜀- to 𝛿-Bismuth Oxide", 《CHIN. PHYS. LETT.》 *
ZHIHUI AI等: "Monoclinic α-Bi2O3 photocatalyst for efficient removal of gaseous NO and HCHO under visible light irradiation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107416899A (en) * 2017-04-05 2017-12-01 河南师范大学 A kind of nano wire α Bi2O3The preparation method of dusty material
CN107416899B (en) * 2017-04-05 2019-01-22 河南师范大学 A kind of nano wire α-Bi2O3The preparation method of dusty material
CN107899602A (en) * 2017-11-01 2018-04-13 河南师范大学 A kind of preparation method with visible light-responded grey basic bismuth nitrate catalysis material
CN107899602B (en) * 2017-11-01 2020-09-18 河南师范大学 Preparation method of gray bismuth subnitrate photocatalytic material with visible light response
CN108927137A (en) * 2018-07-20 2018-12-04 河南师范大学 A kind of preparation method of carbon doping bismuth oxide catalysis material
CN108927137B (en) * 2018-07-20 2021-08-13 河南师范大学 Preparation method of carbon-doped bismuth oxide photocatalytic material

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