CN115893489A - Preparation method and application of bismuth oxyiodide with nonstoichiometric balance iodine atom defects - Google Patents

Preparation method and application of bismuth oxyiodide with nonstoichiometric balance iodine atom defects Download PDF

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CN115893489A
CN115893489A CN202211610767.7A CN202211610767A CN115893489A CN 115893489 A CN115893489 A CN 115893489A CN 202211610767 A CN202211610767 A CN 202211610767A CN 115893489 A CN115893489 A CN 115893489A
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bismuth oxyiodide
iodine atom
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张盾
徐雪磊
王毅
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Institute of Oceanology of CAS
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Abstract

The invention belongs to the field of photocatalysis, and particularly relates to a preparation method and application of bismuth oxyiodide with iodine atom defects in non-stoichiometric balance. The pH value of the bismuth oxyiodide powder synthetic solution is adjusted at room temperature and normal pressure by a wet chemical method, so that the bismuth oxyiodide powder with different iodine content defects can be controllably prepared. The bismuth oxyiodide powder lacking iodine causes the change of the energy band structure of the bismuth oxyiodide due to the lack of iodine atoms, so that the bismuth oxyiodide shows different colors and visible light absorption capability. The deletion of iodine atoms enables the bismuth oxyiodide to have more negative surface charge property, higher specific surface area and photogenerated carrier separation efficiency. Under the irradiation of visible light, the iodine atom-deficient bismuth oxyiodide can generate stronger superoxide, hydroxyl free radicals and cavities to degrade organic pollutants and kill bacteria in a water environment. The method has the advantages of simple process, no need of complex operation, easy control and low cost, and effectively improves the performance of the bismuth oxyiodide.

Description

Preparation method and application of bismuth oxyiodide with nonstoichiometric balance iodine atom defects
Technical Field
The invention belongs to the field of photocatalysis, and particularly relates to a preparation method and application of bismuth oxyiodide with iodine atom defects in non-stoichiometric balance.
Background
In the past decades, visible light induced semiconductor photocatalysts have received wide attention for their potential applications in energy conversion and environmental purification. Bismuth oxyhalides (BiOX, X = F, cl, br and I) are a new class of ternary oxide photocatalysts with a unique layered structure of [ Bi 2 O 2 ] 2+ The plate is characterized. The investigator believes that [ Bi ] 2 O 2 ] 2+ The internal electrostatic field between the plates and the halogen plate is favorable for the separation of photo-generated electron-hole pairs, thereby improving the photocatalysis.
Among these BiOX catalysts, biOI is of great interest for its smallest bandgap (about 1.8 eV) and for its strong absorption in the visible region. However, the BiOI material has low conduction band position and low conductivity, so that the recombination probability of photo-generated electron-hole pairs is high, and the practical application of the BiOI material is limited to a certain extent. Many researchers have been working on finding effective strategies to improve the catalytic activity of the BiOI crystal, such as heterojunction recombination, exposure of specific crystal faces, regulation of morphological structure, and the like. These strategies focus on improving the performance of the photocatalyst, without tuning the intrinsic properties of the BiOI (such as low conductivity, which is critical for charge separation in photocatalysis). Recently, a strategy for iodine atom deficiency has been devised to form new photocatalysts by manipulation of the atomic structure of the BiOI. The resulting iodine-deficient BiOI crystal structure is uniform and has some significantly attractive properties, such as a significantly higher photoconductivity than that of the parent BiOI. In addition, the top of the valence band of BiOI is mainly formed by I 5p And O 2p Hybrid orbit, the bottom of conduction band is mainly Bi 6p The track composition, the change of the ratio of Bi to O to I can adjust samples with energy band structures with different reduction potentials and oxidation potentials. Although at present much multiplexingThe method has succeeded in synthesizing the iodine-deficient BiOI, but the operation of the method usually requires a long-time reaction at high temperature and high pressure. These limitations are detrimental to further industrial applications of the material. It remains challenging to design a simple and effective wet-chemical aqueous phase synthesis strategy at atmospheric pressure for the synthesis of a range of iodine atom deficient BiOIs.
Disclosure of Invention
The invention aims to provide a method for preparing bismuth oxyiodide powder with nonstoichiometric balance iodine atom defects at room temperature and normal pressure and application.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for preparing bismuth oxyiodide powder having nonstoichiometric balance of iodine atom defects at room temperature and normal pressure by wet chemical method at room temperature and normal pressure by adjusting bismuth nitrate (Bi (NO) 3 ) 3 ·5H 2 O) solution and potassium iodide (KI) solution are mixed to obtain the pH value of the precursor solution, and bismuth oxyiodide powder with iodine atom defects is obtained.
Bi (NO) in the precursor solution 3 ) 3 ·5H 2 O solution and KI solution according to the ratio of Bi: i = 1:1.
The Bi (NO) 3 ) 3 ·5H 2 The O solution is prepared by mixing Bi (NO) 3 ) 3 ·5H 2 Dissolving O in glycol solution, and magnetically stirring for 15-20 min; the KI solution is potassium iodide dissolved in deionized water and is magnetically stirred for 15-20 min.
Said separately obtaining Bi (NO) 3 ) 3 ·5H 2 After the O solution and the KI solution, bi (NO) is added 3 ) 3 ·5H 2 And rapidly pouring the O solution into the KI solution under the stirring condition to form a mixed precursor solution, and then adjusting the pH of the solution.
The pH value of the mixed precursor solution is adjusted by adopting a NaOH saturated aqueous solution, and the NaOH aqueous solution is quickly dripped to adjust the pH value of the mixed precursor solution to 2-9. With the increasing of the pH value, the content of iodine atom defects in the obtained bismuth oxyiodide powder is gradually increased.
The bismuth oxyiodide with iodine atom defects prepared by adjusting different pH values is quickly centrifugally cleaned for 3-6 times by using deionized water, and then dried in an oven at the temperature of 60-80 ℃ for 12-24 hours for later use.
The bismuth oxyiodide with the iodine atom defect which is not stoichiometrically balanced is prepared by the method, and the bismuth oxyiodide with the iodine atom defect which is not stoichiometrically balanced is obtained by different colors, sheets or petals which are piled up according to the method.
The use of bismuth oxyiodide having a non-stoichiometrically balanced iodine atom defect as a photocatalyst for degrading organic contaminants and/or sterilizing in a water purification environment.
The principle of the invention is as follows: by Bi (NO) 3 ) 3 ·5H 2 BiI in O and KI mixed precursor solution 3 +H 2 O→BiOI+2H + +2I - And (3) carrying out Ostwald ripening reaction, and quickly preparing the BiOI crystal material with balanced stoichiometry in the mixed precursor solution. Then NaOH solution is quickly dripped into the mixed precursor solution, because xBiOI +4OH - →Bi x O x+2 I (x-4) +4I - +2H 2 And (4) O reaction, namely replacing iodine atoms in the BiOI into the solution to form the BiOI with nonstoichiometric equilibrium iodine atom defects. After the iodine atom structure defect is introduced into the BiOI, the photoproduction current density of the bismuth oxyiodide is obviously improved, and the conduction band and the valence band of the crystal are deviated, so that the BiOI has better oxidation-reduction activity. The photocatalytic activity is obviously improved, so that the BiOI can generate more reactive active substances, and the water body environment is obviously purified.
The invention has the advantages of
The invention adopts a wet chemical method to prepare the BiOI with the structural defect at the room temperature and the room pressure. Firstly, the preparation conditions overcome the high-temperature and high-pressure environment required by the defects of the traditional structure, so that the preparation of the BiOI has more convenience and practical operability. And the iodine atom defect is adjusted to act on the structure of the BiOI, so that the separation and transfer efficiency of a photon-generated carrier of the BiOI can be effectively improved, and the BiOI heterojunction has higher photocatalytic activity compared with the BiOI heterojunction.
Drawings
Fig. 1 is an electron photograph of bismuth oxyiodide powder with a series of iodine atom defects provided by the embodiment of the invention.
Fig. 2 is an XRD spectrum of bismuth oxyiodide powder with a series of iodine atom defects provided by the embodiments of the present invention.
Fig. 3 is a TEM spectrum of a bismuth oxyiodide powder with iodine atom defects prepared at pH2.48 and 6 according to an embodiment of the present invention, wherein (a) pH 2.48; (b) pH 6.
FIG. 4 is a UV-vis DRS spectrum of a series of iodine atom deficient bismuth oxyiodide powders provided in accordance with an embodiment of the present invention.
Fig. 5 is a graph of photo-generated current intensity of bismuth oxyiodide powder with a series of iodine atom defects provided by the embodiment of the invention.
FIG. 6 is a Zeta potential diagram of the surface of bismuth oxyiodide powder with a series of iodine atom defects provided by the embodiment of the invention.
Fig. 7 is a kinetic curve diagram of degradation of rhodamine B by bismuth oxyiodide powder with a series of iodine atom defects, provided by an embodiment of the present invention.
FIG. 8 is a photograph showing that the iodine atom-deficient bismuth oxyiodide powder prepared at pH2.48 (a, c) and pH 7 (b, d) according to the embodiment of the present invention kills large intestine (a, b) and Staphylococcus aureus (c, d).
Detailed Description
The present invention is further illustrated by the following specific examples, which are provided to assist those of ordinary skill in the art in more fully understanding the present invention, and are not intended to be limiting in any way. Other changes and modifications can be made according to the technical scheme and the technical idea of the invention, and the changes and modifications still fall within the protection scope covered by the invention.
According to the invention, biOI powder with iodine atom structure defects is quickly synthesized at room temperature and normal pressure by regulating the pH value of a BiOI synthetic solution through a wet chemical method and structure defect engineering, the BiOI lacking iodine atoms has different physicochemical properties, the BiOI with non-stoichiometric balance has higher photocatalytic activity compared with the BiOI with stoichiometric balance, and the powder can simultaneously generate reactive substances such as superoxide, hydroxyl free radicals, cavities and the like in a water environment, so that organic pollutants in a water environment can be degraded, microorganisms can be killed, and the water environment can be purified. The invention has simple process, easy control and low cost. The BiOI with the structural defect prepared by the method has potential application prospects and reference significance in the aspects of buildings, medical treatment, ocean engineering facilities, aquaculture, ship anti-biofouling, water body purification, sterilization and disinfection and the like.
Example 1
(1) Weighing 0.05M Bi (NO) 3 ) 3 ·5H 2 Dissolving the mixture in 500mL of glycol solution, and continuously stirring for 15min to obtain a suspension; 0.05M KI was weighed and dissolved in 500mL deionized water, and stirring was continued for 15min to obtain a clear aqueous solution. The suspension was quickly poured into a clear aqueous solution and stirred under magnetic stirring for 2min to obtain a mixed precursor.
(2) And (3) quickly dropwise adding a saturated NaOH aqueous solution into the mixed precursor solution, and adjusting the pH of the precursor solution to 2.48,3,4,5,6,7,8 and 9 to obtain the BiOI powder under different pH values. At pH 10, bismuth oxyiodide could not be produced due to the absence of iodine atoms.
(3) And respectively centrifugally washing the obtained different BiOI powder for 3 times by using deionized water, and drying the powder for 24 hours in an air blast drying box at the drying condition of 60 ℃ to obtain a series of BiOI powder with iodine atom defect structures in different colors. (see FIG. 1)
As can be seen from a series of electron photographs of the iodine deficient biti powders of fig. 1, the corresponding products have a gradually decreasing color, which is related to a change in their energy band gap (Eg).
Example 2
XRD patterns of a series of iodine-deficient bisi powders obtained in example 1 were observed.
(see FIG. 2)
From the XRD pattern of FIG. 2, it can be seen that the stoichiometric number BiOI obtained by preparation at pH2.48 corresponds to PDF #73-2062. Due to [ Bi ] 2 O 2 ] 2+ The enriched bismuth and oxygen atoms may cause expansion and deformation of the BiOI crystal structure, and thus correspond to the crystal plane at 29.7 DEG(012) Will be lower than the diffraction angle of a defect-free BiOI crystal due to the absence of iodine atoms. And the peak shift position is lower as the iodine deficiency content increases, i.e. the pH increases. In addition to the difference in the positions of the crystallization peaks, the peak intensity of the bisi crystal with iodine atom defects in non-stoichiometric amounts was broader than that of the diffraction peak of the stoichiometric (iodine defect-free) bisi, indicating that the bisi crystal with iodine atom defects had more and smaller crystal units. This is advantageous in improving the activity of the photocatalyst per unit area.
Example 3
TEM observations were made of the iodine-deficient bisi powders obtained in example 1, prepared at ph2.48 and 6. (see FIG. 3)
TABLE 1 preparation of bismuth oxyiodide powder interplanar spacing at different pH
Figure BDA0003999517130000041
As can be seen from the TEM image of fig. 3 and table 1, the facets with lattice spacings of 0.281 and 0.201nm with an included angle of 45 ° correspond to the (110) and (020) facets, respectively, of the bio i, and the locally enlarged HRTEM images further show a match with the unit cell of PDF #73-2062 of the bio i. In contrast, HRTEM images of bismuth oxyiodide deficient in iodine atoms after pH adjustment by NaOH solution showed wider lattice fringe spacing for the (110) and (020) crystal planes than the stoichiometric bisi, mainly due to the change in electric field within the crystal resulting in expansion of the crystal structure. In the absence of iodine defects, bismuth oxyiodide exhibits a lamellar appearance. At pH >3, iodine atom defects appear, bismuth oxyiodide presents the appearance of petal-like piled spheres, and the spheres become smaller gradually with increasing pH and iodine atom loss.
Example 4
A series of iodine-deficient bisi powders obtained as prepared in example 1 were observed for their visible light absorption properties. (see FIG. 4)
With BaSO 4 For a reference sample (U-4100, hitachi, japan), the visible light absorption characteristics thereof were analyzed using an ultraviolet-visible diffuse reflectance absorption apparatus (UV-vis DRS) equipped with an integrating sphere.
As can be seen from the UV-vis DRS spectrum of the photocatalytic composite film in fig. 4, the absorption boundary of the bio i powder is significantly reduced with increasing pH, i.e., the number of structural defects of iodine atoms, and the powder exhibits gradually decreasing visible light absorption properties.
Example 5
A series of iodine-deficient biti powders prepared in example 1 were tested for their photo-generated current properties, as well as for their non-iodine atom-deficient bitoi powders. (see FIG. 5)
The PEC performance of different bisi powders was investigated by measuring their transient photoproduction current response performance under LED illumination. The BiOI powder without iodine atom defects has a relatively narrow band gap (1.77 eV), so that the photogenerated current is relatively weak, i.e., photogenerated carriers are easily recombined. Surprisingly, the photoproduction current response of the powder was significantly improved, about 2 times higher than that of the original BiOI, after the introduction of the iodine atom structural defects in the BiOI, probably due to the presence of iodine vacancies regulating the electron density, which in turn improves the separation and transport efficiency of the photoproducted holes and electrons, which in turn improves the PEC performance.
Example 6
A Zeta potential test was performed on a series of iodine deficient biti powders obtained by the preparation of example 1.
(see FIG. 6)
The photocatalytic activity of the photocatalyst is closely related to the interface function and electronic performance of the photocatalyst. The stoichiometric BiOI powder showed a Zeta potential of 0.98 + -0.23 eV. In contrast, the Zeta potential of BiOI powder (pH 3) containing structural defects of iodine atoms is much lower, 0.87. + -. 0.06eV. Interestingly, at pH 4, the surface potential of the BiOI powder reversed to a lower Zeta potential, i.e., surface electronegativity. This indicates that the BiOI containing iodine atom defects has a higher internal electric field strength and can more effectively drive the separation and transfer of photo-generated charges.
In conclusion, the bismuth oxyiodide crystal powder obtained by the method has a series of iodine-deficient BiOI powders at room temperature and normal pressure, and the main crystal face spacing of the bismuth oxyiodide is increased due to the existence of the iodine atom structure defect. Although the iodine atom defect causes a decrease in the visible light absorption ability, bismuth oxyiodide having an iodine atom defect exhibits higher photocarrier separation efficiency, i.e., better photocatalytic activity, due to the band gap broadening and the increase in internal electric field intensity. The electronegativity of the surface of the bismuth oxyiodide powder containing iodine atom defects is favorable for absorbing positively charged pollutants, namely the bismuth oxyiodide powder has a high removing effect on positively charged organic pollutants on the surface;
application example 1
A series of iodine deficient biai powders prepared in example 1 were subjected to a degraded rhodamine B (RhB) performance test.
30mL of 10mg/L RhB solution were added to each glass bottle to obtain iodine-deficient BiOI powder at different pH. Before illumination, the glass bottle is placed in a dark environment for 30min to establish adsorption-desorption balance of RhB on the powder surface. At certain time intervals, 100. Mu.L of the reaction solution was pipetted onto a 96-well transparent plate, and the absorbance value of RhB at 554nm was measured using a microplate reader to determine the degradation kinetic curve of RhB (see FIG. 7).
From the observation of fig. 7, it can be found that the BiOI powder having a high content of structural defects of iodine atoms can remove RhB more effectively. Obviously, a large number of active adsorption sites and adsorption force exist between the molecules of the electropositive RhB dye and the photocatalysts with electronegativity, so that the RhB dye can be quickly adsorbed on the BiOI powder obtained by the structural defects of iodine atoms.
Meanwhile, rhodamine B is degraded by using the BiOI powder which is described in the prior document and is lack of iodine in the manner, and the bismuth oxyiodide which is prepared by the method and has iodine defects shows higher removal efficiency under lower light irradiation intensity and time at the same content of photocatalyst powder and RhB, as shown in Table 2.
TABLE 2 preparation of bismuth oxyiodide powder for RhB degradation efficiency under different references
Figure BDA0003999517130000061
[1]Pei Wu,Li Feng,Yicong Liang,Xia Zhang,Xuhao Li,Shenghai Tian,Hai Hu,Gaohong Yin,Sarfaraz Khan,Large-scale synthesis of 2D bismuth-enriched bismuth oxyiodidesat low temperatures for high-performance supercapacitorand photocatalytic applications,Journal of materials science:materials in electronics,2020(31)5385-5401.
[2]Gongjuan Wu,Yan Zhao,Yawen Li,Hongmei Ma,Jingzhe Zhao,pH-dependent synthesis of iodine-deficient bismuth oxyiodidemicrostructures:Visible-light photocatalytic activity,Journal of colloid and interface science,2018(510)228-236.
[3]Quancheng Liu,Dekun Ma,Yingying Hu,Yawen Zeng,Shaoming Huang,Various bismuth oxyiodidehierarchical architectures:alcohothermal-controlled synthesis,photocatalytic activities,andadsorption capabilities for phosphate in water,ACS applied materials interfaces,2013(5)11927-11934.
Application example 2
Experiments for killing escherichia coli and staphylococcus aureus were performed on the iodine atom-deficient bisi powder prepared at pH2.48 and pH 7 in example 1 as photocatalytic powder.
In normal times, E.coli was stored in glycerol at-20 ℃. For experimental work, 2mL of E.coli was removed from the glycerol medium and cultured in 250mL of sterile LB medium with stirring (180 rpm/min) at 37 ℃ for 20. + -.1 h. The bacteria were harvested by centrifugation (4500 rpm,15 minutes) and resuspended in sterile distilled water to give a "standard bacterial suspension" of E.coli and S.aureus of 5.06. + -. 0.08X 10 8 And 2.67. + -. 0.07X 10 8 CFU/mL, and further diluted to 10 5 CFU/mL。
In a typical test procedure, all photocatalytic films and quartz tubes were irradiated with ultraviolet rays for 24 hours before the photocatalytic killing test of E.coli to avoid the influence of bacteria in the atmosphere. 30mL of a standard bacterial suspension and 30mg of the above different photocatalyst powders were added to a quartz tube, and the suspension was exposed to visible light (PCX 50C Discover, beijing Pofely science Co., ltd., china). 100. Mu.L of the suspension was dropped onto LB agar plates at 3 hours, and incubated at 37 ℃ for 24 hours to observe the number of bacteria. (see FIG. 8)
From the results of FIG. 8, it can be seen that BiOI with a defect in the structure of iodine atom showed higher photocatalytic inactivation activity for Escherichia coli and Staphylococcus aureus, and colonies were not substantially observed on LB plate. Indicating that the sterilizing capability of the BiOI with the iodine atom structure defect is more than 99.99 percent.

Claims (8)

1. A method for preparing bismuth oxyiodide with non-stoichiometric balance iodine atom defects is characterized by comprising the following steps: by conditioning bismuth nitrate (Bi (NO) by wet chemical method at room temperature and pressure 3 ) 3 ·5H 2 O) solution and potassium iodide (KI) solution are mixed to obtain the pH value of the precursor solution, and the bismuth oxyiodide powder with iodine atom defects is obtained.
2. The process for producing bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects according to claim 1, wherein: bi (NO) in the precursor solution 3 ) 3 ·5H 2 O solution and KI solution according to the ratio of Bi: i = 1:1.
3. The process for producing bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects according to claim 1 or 2, wherein: the Bi (NO) 3 ) 3 ·5H 2 The O solution is prepared by mixing Bi (NO) 3 ) 3 ·5H 2 Dissolving O in glycol solution, and magnetically stirring for 15-20 min; the KI solution is potassium iodide dissolved in deionized water and is magnetically stirred for 15-20 min.
4. A process for preparing bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects according to claim 3, wherein: said separately obtaining Bi (NO) 3 ) 3 ·5H 2 After the O solution and the KI solution, bi (NO) is added 3 ) 3 ·5H 2 And quickly pouring the O solution into the KI solution under the stirring condition to form a mixed precursor solution, and then adjusting the pH of the solution.
5. The process for producing bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects according to claim 4, wherein: the pH value of the mixed precursor solution is adjusted by adopting a NaOH saturated aqueous solution, and the NaOH aqueous solution is quickly dripped to adjust the pH value of the mixed precursor solution to 2-9.
6. The process for producing bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects according to claim 4, wherein: the bismuth oxyiodide with iodine atom defects prepared by adjusting different pH values is quickly centrifugally cleaned for 3-6 times by using deionized water, and then dried in an oven at the temperature of 60-80 ℃ for 12-24 hours for later use.
7. A bismuth oxyiodide having a nonstoichiometric balance of iodine atom defects, prepared by the process of claim 1, wherein: bismuth oxyiodide having non-stoichiometrically balanced iodine atom defects in spherical, differently colored, flake-like or petal-like packing obtained by the method of claim 1.
8. Use of bismuth oxyiodide having a non-stoichiometrically balanced iodine atom defect according to claim 7, wherein: the bismuth oxyiodide with the structural defect and the iodine atom defect is applied to the water purification environment as a photocatalyst for degrading organic pollutants and/or sterilizing.
CN202211610767.7A 2022-12-14 2022-12-14 Preparation method and application of bismuth oxyiodide with nonstoichiometric balance iodine atom defects Pending CN115893489A (en)

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