CN105523584A - Bi2O2CO3 nanocrystal with unique morphology, and preparation method thereof - Google Patents

Bi2O2CO3 nanocrystal with unique morphology, and preparation method thereof Download PDF

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Publication number
CN105523584A
CN105523584A CN201410512422.7A CN201410512422A CN105523584A CN 105523584 A CN105523584 A CN 105523584A CN 201410512422 A CN201410512422 A CN 201410512422A CN 105523584 A CN105523584 A CN 105523584A
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reaction
bi2o2co3
nanocrystal
nanocrystalline
preparation
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韩巧凤
杨丽丽
赵靳
汪信
朱俊武
武晓东
卑凤利
刘孝恒
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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Abstract

The invention discloses a Bi2O2CO3 nanocrystal with a unique morphology, and a preparation method thereof. According to the invention, bismuth citrate (C6H5BiO7) is adopted as a raw material; a dilute ammonia water solution is adopted as a solvent; and the hemispherical-structured Bi2O2CO3 nanocrystal composed of wound nano-sheets with curl edges is prepared with a hydrothermal method. The preparation method of the Bi2O2CO3 nanocrystal comprises the following steps: C6H5BiO7 is dissolved in the dilute ammonia water solution; the solution is subjected to a reaction in a reaction kettle; when the reaction is finished, washing is carried out, such that the hemispherical Bi2O2CO3 nanocrystal is obtained. The Bi2O2CO3 nanocrystal obtained through the reaction has a unique morphology and high specific surface area. With the Bi2O2CO3 nanocrystal, material performance can be effectively improved. In a photocatalysis performance test, the product obtained with the method shows good RhB catalytic degradation activity, which shows that the product has good application prospect in the respect of pollutant photocatalytic degradation.

Description

A kind of Bi of unique morphology 2o 2cO 3nanocrystalline and preparation method thereof
Technical field
The present invention relates to Bi 2o 2cO 3nanocrystalline and preparation method thereof, the particularly Bi of unique morphology 2o 2cO 3nanocrystalline and preparation method thereof, belong to field of inorganic nano-material preparation.
Background technology
As everyone knows, the physics and chemistry character of nano material and the microtexture of material closely related, comprise size, pattern and specific surface area etc., therefore, due to the excellent properties of laminate structure, the fields such as electricity, magnetics, catalysis and medical science are widely used in.Because nano level unitized construction can show new or better properties, low-dimensional (0D, 1D or 2D) nano-scale self-assembly (such as, nano particle, nano wire, nano belt and nanometer sheet) more and more paid attention to the nano-micro structure of three-dimensional (3D) layering.
Along with industrial expansion, waste water from dyestuff has become main environmental pollutant, TiO 2present research emphasis is become Deng conductor photocatalysis.In these photocatalysts, bismuthino compound is (as Bi 2wO 6, Bi 4ti 3o 12, BiOX (X=Cl, Br, I) etc.) and due to its higher photocatalytic activity, become the emphasis of research.Due to (Bi 2o 2) 2+easy accumulation or all belonged to stratiform or Aurivillius related compound, same Bi by these bismuthino compounds of template as other atoms or group 2o 2cO 3also easily form the 3D flower-like structure of flake-assembly mode, and replace haloid element poisonous in BiXO (X=Cl, Br, I) due to it by more green element (C, O), novel photocatalyst material may be become.
Bi 2o 2cO 3have good photocatalysis performance, the people such as JialeTang adopts with bismuth citrate and urea for raw material, and N.F,USP MANNITOL is as solvent, and at 150 DEG C, hydro-thermal obtains Bi 2o 2cO 3; The people such as PuttaswamyMadhusudan for raw material, add PVP as tensio-active agent with bismuth and ammonium citrate, urea and sodium-acetate, and at 180 DEG C, hydro-thermal obtains Bi 2o 2cO 3.Although obtained Bi 2o 2cO 3be the flower-like structure that nanometer sheet assembling is formed, but owing to adding organic solvent or tensio-active agent in preparation process, preparation process still can cause burden to environment and tensio-active agent is not easily cleaned, and therefore this method is unfavorable for commercial introduction.
Summary of the invention
The object of the present invention is to provide a kind of Bi 2o 2cO 3nanocrystalline and preparation method thereof.
The technical solution realizing the object of the invention is: a kind of Bi of unique morphology 2o 2cO 3nanocrystalline, described Bi 2o 2cO 3nanocrystalline be edge curl nanometer sheet be wound around composition hemisphere.
Soft chemical method is utilized to prepare the above-mentioned Bi with unique morphology 2o 2cO 3nanocrystalline method, comprises the following steps:
Step one: by C 6h 5biO 7be dissolved in dilute ammonia solution and make mixing solutions;
Step 2: step 2 solution is placed in reaction kettle for reaction;
Step 3: reaction terminates the hemispherical Bi that namely rear washing obtains the nanometer sheet winding composition of edge curl 2o 2cO 3nanocrystalline.
C in gained mixing solutions in step one 6h 5biO 7volumetric molar concentration be 0.067mol/L, the volume fraction of dilute ammonia solution is 17%.
Temperature of reaction described in step 2 is 180 DEG C, and the reaction times is 12h.
Compared with prior art, the present invention has following remarkable advantage:
1, method is simple, without the need to adding any catalyzer and tensio-active agent, only uses bismuth citrate namely to obtain Bi for raw material 2o 2cO 3nanocrystalline;
2, environmentally safe, does not use any organic solvent in preparation process, is only that namely solvent obtains Bi with dilute ammonia solution 2o 2cO 3nanocrystalline;
3, obtained Bi 2o 2cO 3nanocrystalline products is the hemisphere of the nanometer sheet winding composition of edge curl, has larger specific surface area, is conducive to the raising of its performance;
4, pass through this Bi 2o 2cO 3nanocrystalline photocatalysis performance carries out test and finds, nanocrystallinely shows excellent photocatalysis performance to RhB, and after circulation 5 times its photocatalysis effect and pattern substantially constant, show the equal quite stable of its stuctures and properties.
Accompanying drawing explanation
Fig. 1 is the Bi that hydrothermal method of the present invention preparation has unique morphology 2o 2cO 3nanocrystalline schematic flow sheet.
Fig. 2 is obtained Bi 2o 2cO 3tEM and SEM figure: (a) embodiment 1; B () is through 5 circulation degradeds; (c) comparative example 1, illustration is comparative example 2; (d) comparative example 3.
Fig. 3 is the flower-shaped Bi that comparative example 4 obtains 2o 2cO 3sEM figure.
Fig. 4 (a) is the degradation rate comparison diagram of two kinds of patterns; (b) hemispherical Bi 2o 2cO 35 times circulation degraded figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Composition graphs 1, the present invention utilizes dilute ammonia solution to have the Bi of unique morphology for solvent preparation 2o 2cO 3nanocrystalline method, its feature comprises the following steps:
Step one: by C 6h 5biO 7be dissolved in dilute ammonia solution, wherein C 6h 5biO 7volumetric molar concentration be 0.067mol/L, the volume fraction of dilute ammonia solution is 17%;
Step 2: step one solution is placed in reaction kettle for reaction, wherein temperature of reaction is 180 DEG C, and the reaction times is 12h;
Step 3: reaction terminates rear washing and namely obtains hemispherical Bi 2o 2cO 3nanocrystalline.
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described in detail:
Embodiment 1:
Step one: by 2mmolC 6h 5biO 7being dissolved in 30mL volume fraction is in the dilute ammonia solution of 17%;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 180 DEG C, the reaction times is 12h;
Step 3: namely obtain Bi after product washing step 2 obtained 2o 2cO 3nanocrystalline.
Products therefrom, as shown in 2 (a), can be found out by TEM figure and illustration SEM figure, and product morphology is the hemisphere of the nanometer sheet winding composition of edge curl, and the nanometer sheet thickness of composition hemisphere is about about 15nm.Fig. 2 (b) is the TEM figure of sample after 5 circulation degradeds, can find that sample topography is substantially constant; For hemispherical configuration circulates, (photochemical catalysis all uses 10mgBi to Fig. 4 (b) under 300W mercury lamp for the photocatalytic activity figure of 5 times 2o 2cO 3degraded 5mg/LRhB solution), as can be seen from the figure the degradation rate of 5 circulations is substantially identical, shows that it has good optical stability.
Comparative example 1:
Step one: by 2mmolC 6h 5biO 7being dissolved in 30mL volume fraction is in the dilute ammonia solution of 17%;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 180 DEG C, the reaction times is 6h;
Step 3: namely obtain Bi after product washing step 2 obtained 2o 2cO 3nanocrystalline.
Shown in the transmission electron microscope picture 2 (c) of products therefrom, because nanocrystal surface has many particle depositions to be spherical.
Comparative example 2:
Step one: by 2mmolC 6h 5biO 7being dissolved in 30mL volume fraction is in the dilute ammonia solution of 17%;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 180 DEG C, the reaction times is 9h;
Step 3: namely obtain Bi after product washing step 2 obtained 2o 2cO 3nanocrystalline.
Shown in transmission electron microscope picture 2 (c) illustration of products therefrom, product is the ball-like structure of nanometer sheet composition, but and the size of nanometer sheet is less.
Comparative example 3:
Step one: by 2mmolC 6h 5biO 7being dissolved in 30mL volume fraction is in the dilute ammonia solution of 17%;
Step 2: by the isothermal reaction in closed reactor of the solution of step one gained, temperature of reaction 180 DEG C, the reaction times is 24h;
Step 3: namely obtain Bi after product washing step 2 obtained 2o 2cO 3nanocrystalline.
Shown in the transmission electron microscope picture 2 (d) of products therefrom, product is the irregular coacervate of nanometer sheet.
Comparative example 4:
Step one: by 2mmolC 6h 5biO 7be dissolved in 5mLNH 3h 2in O;
Step 2: add 25mLEG in step one solution,
Step 3: by the isothermal reaction in closed reactor of the solution of step 2 gained, temperature of reaction 180 DEG C, the reaction times is 12h;
Step 4: namely obtain Bi after product washing step 3 obtained 2o 2cO 3nanocrystalline.
Figure 3 shows that the flower-shaped Bi that comparative example is obtained 2o 2cO 3nanocrystalline SEM figure; Fig. 4 (a) is two kinds of pattern Bi 2o 2cO 3photocatalytic activity comparison diagram, far above flower-like structure, (photochemical catalysis all uses 10mgBi to the degradation rate of as can be seen from the figure hemispherical configuration under 300W mercury lamp 2o 2cO 3degraded 5mg/LRhB solution).

Claims (4)

1. the Bi of a unique morphology 2o 2cO 3nanocrystalline, it is characterized in that, described Bi 2o 2cO 3nanocrystalline be edge curl nanometer sheet be wound around composition hemisphere.
2. the Bi of a unique morphology as claimed in claim 1 2o 2cO 3nanocrystalline preparation method, is characterized in that, comprises the following steps:
Step one: by C 6h 5biO 7be dissolved in dilute ammonia solution and make mixing solutions;
Step 2: step 2 solution is placed in reaction kettle for reaction;
Step 3: reaction terminates the hemispherical Bi that namely rear washing obtains the nanometer sheet winding composition of edge curl 2o 2cO 3nanocrystalline.
3. the Bi of unique morphology according to claim 1 2o 2cO 3nanocrystalline preparation method, is characterized in that, C in gained mixing solutions in step one 6h 5biO 7volumetric molar concentration be 0.067mol/L, the volume fraction of dilute ammonia solution is 17%.
4. the Bi of unique morphology according to claim 1 2o 2cO 3nanocrystalline preparation method, is characterized in that, the temperature of reaction described in step 2 is 180 DEG C, and the reaction times is 12h.
CN201410512422.7A 2014-09-29 2014-09-29 Bi2O2CO3 nanocrystal with unique morphology, and preparation method thereof Pending CN105523584A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112642458A (en) * 2020-12-23 2021-04-13 陕西科技大学 Heterojunction photocatalyst and preparation method and application thereof
CN115196673A (en) * 2022-07-04 2022-10-18 西北大学 Polycrystalline phase Bi 2 O 3 Material, preparation method and application

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CN102275987A (en) * 2011-05-25 2011-12-14 中国地质大学（武汉） Nano/micro-scale sheet bismuthyl carbonate material and preparation method thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112642458A (en) * 2020-12-23 2021-04-13 陕西科技大学 Heterojunction photocatalyst and preparation method and application thereof
CN115196673A (en) * 2022-07-04 2022-10-18 西北大学 Polycrystalline phase Bi 2 O 3 Material, preparation method and application
CN115196673B (en) * 2022-07-04 2024-02-20 西北大学 Polycrystalline Bi 2 O 3 Material, preparation method and application

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