CN115025784B - CoOx/BiVO 4 Nanosheets, preparation method and application thereof - Google Patents

CoOx/BiVO 4 Nanosheets, preparation method and application thereof Download PDF

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CN115025784B
CN115025784B CN202210679053.5A CN202210679053A CN115025784B CN 115025784 B CN115025784 B CN 115025784B CN 202210679053 A CN202210679053 A CN 202210679053A CN 115025784 B CN115025784 B CN 115025784B
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bivo
solution
coo
nano
sheet
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CN115025784A (en
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孙秀云
李昊霖
胡雅
陆静宇
诸葛凯悦
孙鹏
李健生
沈锦优
韩卫清
刘晓东
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Nanjing University of Science and Technology
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Abstract

The invention discloses a CoOx/BiVO 4 A nano-sheet, a preparation method and application thereof belong to the field of semiconductor materials. The method prepares BiVO through hydrothermal reaction 4 When the catalyst is used, the lower temperature (1111111 ℃) and the shorter reaction time (51171 min) are adopted, so that the preparation time is shortened, meanwhile, good nano-sheet morphology can be formed, the specific surface area of the catalyst is obviously increased, more adsorption sites and active sites are provided, and the photocatalytic performance is improved; meanwhile, absolute ethyl alcohol is selected as the impregnating solution, so that the drying time is shortened, the composite material has narrower band gap width, the visible light utilization capacity of the composite material is improved, and the photo-generated carrier separation effect of the composite material is better.

Description

CoOx/BiVO 4 Nanosheets, preparation method and application thereof
Technical Field
The invention belongs to the field of semiconductor materials, and in particular relates to a CoO x /BiVO 4 A nano-sheet and a preparation method and application thereof.
Background
BiVO 4 Is a common n-type semiconductor photocatalytic material, and mainly has three crystal structures: tetragonal scheelite type, tetragonal zircon type and monoclinic scheelite type. The monoclinic scheelite type has the advantages of narrow band gap width, good stability, no toxicity and the like. However, pure BiVO 4 The energy gap is narrower, so that the photon-generated carrier recombination probability is higher, and the photocatalysis performance is required to be further improved.
To improve BiVO 4 Photo-catalytic performance, biVO is commonly controlled by morphology regulation, semiconductor compounding and other methods in the prior art 4 And (5) modifying. In improving BiVO 4 Among the various methods of photocatalytic performance, the construction of p-n heterostructures is considered to be the most effective method of improving photocatalyst activity. CoO (CoO) x As an important p-type semiconductor material, the material has the advantages of low cost, no toxicity, good stability and the like, and has good application prospect in the field of photocatalysis. Due to CoO x And BiVO 4 Band structure matching, coO x Can be combined with BiVO 4 Forming a p-n heterostructure to make the photo-generated electrons in the BiVO 4 Surface enrichment, photo-generated holes in CoO x The surface is enriched, and the carrier separation rate is improved, so that the photocatalytic performance is improved.
The Chinese patent publication No. CN109794256A discloses a preparation method and application of bismuth vanadate composite material loaded with cobalt oxide nano particles, which comprises the following steps of BiVO 4 Soaking the film in CoCl 2 The solution is put into the solution for 10 to 12 hours to lead Co to be formed by 2+ Reaching adsorption balance; then Co is adsorbed 2+ BiVO of (C) 4 Drying the film in a drying oven, placing in a muffle furnace, and calcining at 450-500 ℃ for 4-5 h to obtain the loaded CoO x BiVO of (C) 4 Film CoO x /BiVO 4 . The preparation time is about 14-17 h, and the high-temperature calcination at 450-500 ℃ is needed. Calcining for longer time and higher temp. with higher energy consumption, resulting in higher catalyst performancePreparation costs, and may result in BiVO 4 Agglomeration occurs, destroying its own structure, resulting in a decrease in photocatalytic performance.
This patent discloses a CoO x /BiVO 4 The nano-sheet preparation method has the advantages that the composite material prepared by the method has a narrower band gap and good visible light utilization performance, and photo-generated carriers can be effectively separated, so that the BiVO is effectively improved 4 Is used for the photocatalytic performance of the catalyst.
Disclosure of Invention
1. Problems to be solved
The present invention is directed to CoO in the prior art x /BiVO 4 In the preparation process of (2), the problems of high energy consumption and insufficient catalytic performance of the final product caused by longer preparation time and high temperature are solved, and a CoO is provided x /BiVO 4 A nano-sheet and a preparation method and application thereof.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention provides a CoO x /BiVO 4 A method of preparing a nanoplatelet, the method comprising the steps of:
s1: bi (NO) 3 ) 3 ·5H 2 O and SDBS (sodium dodecyl benzene sulfonate) are dissolved in HNO 3 Obtaining a solution A in the solution; NH is added to 4 VO 3 Dissolving in NaOH solution to obtain solution B; dropwise adding the solution B into the solution A, regulating the pH of the solution to 6-7, and uniformly stirring to obtain a precursor solution;
s2: carrying out hydrothermal reaction on the precursor liquid in the step S1 at 160-200 ℃ for 50-70 min to obtain yellow precipitate; washing the yellow precipitate with water, washing with alcohol, and oven drying to obtain BiVO 4 ；
S3: biVO in S2 4 And Co (NO) 3 ) 2 ·6H 2 Dissolving O in ethanol, uniformly dispersing by ultrasonic waves, and drying; calcining the dried sample in a muffle furnace at 180-220 ℃ for 0.8-2.0 h to obtain CoO x /BiVO 4 A nano-sheet.
Preferably, bi (NO 3 ) 3 ·5H 2 O andNH in solution B 4 VO 3 The molar concentrations are the same.
Preferably, bi (NO 3 ) 3 ·5H 2 The molar concentration of O is 0.2-0.34 mmol/mL. Further, bi (NO 3 ) 3 ·5H 2 The molar concentration of O was 0.27mmol/mL.
Preferably, the above-mentioned Bi (NO) in S1 is 1mmol relative to 1mmol 3 ) 3 ·5H 2 The dosage of O and SDBS is 0.125-0.375 g. Still further, the SDBS was used in an amount of 0.25g.
Preferably, the HNO in S1 is 4M 3 Solution, 2M NaOH solution.
Preferably, in the step S1, the solution B is dropwise added into the solution A by using a peristaltic pump, and the rotation speed of the peristaltic pump is 70-90 r/min. Still further, the peristaltic pump speed is 80r/min.
Preferably, the stirring in S1 is uniform by a magnetic stirrer.
Preferably, the hydrothermal reaction temperature in the step S2 is 180 ℃ and the reaction time is 1h.
Preferably, in the above S3, biVO is provided with respect to 1mL of ethanol 4 The amount of (C) is 5-15 mg, co (NO) 3 ) 2 ·6H 2 The dosage of O is 0.25-0.75 mg. Further, biVO 4 Is 10mg, co (NO) 3 ) 2 ·6H 2 The amount of O used was 0.25mg.
Preferably, the calcination temperature in the above step S3 is 200℃and the time is 2 hours.
The invention also provides a CoO x /BiVO 4 The nano-sheet is prepared by the preparation method.
The invention also provides the CoO x /BiVO 4 Application of nanosheets or preparation method to CoO x /BiVO 4 The nanosheets are used for photoelectrocatalysis.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention provides a CoO x /BiVO 4 Method for preparing nanosheets, theMethod for preparing BiVO through hydrothermal reaction 4 In the process, a lower temperature (160-200 ℃) and a shorter reaction time (50-70 min) are used, so that the preparation time is shortened, and meanwhile, a good nano-sheet morphology can be formed, because a higher hydrothermal temperature and a longer reaction time can possibly lead to BiVO in the solution 4 Ostwald ripening occurs, agglomeration forms a block structure, and the nano-sheet morphology can remarkably increase the specific surface area of the catalyst, and more adsorption sites and active sites are provided, so that the photocatalytic performance is improved.
(2) The invention provides a CoO x /BiVO 4 According to the preparation method of the nano-sheet, absolute ethyl alcohol is selected as the impregnating solution, so that the drying time is shortened, the composite material obtains narrower band gap width, the visible light utilization capacity of the composite material is improved, and the photo-generated carrier separation effect of the composite material is better. As can be seen from FIG. 1, coO is prepared by selecting ethanol as the impregnating solution x /BiVO 4 The diffraction peak intensity of the nano-sheet is higher than that of CoO prepared by using water as impregnating solution x /BiVO 4 The nanosheets are weaker, presumably because ethanol as the impregnating solution may enhance CoOx in BiVO 4 Is of a dispersity of (3). Thus, coO prepared by using ethanol as the impregnating solution x /BiVO 4 The nano-sheet has better photocatalysis effect.
Drawings
FIG. 1 is a pure BiVO prepared according to the present invention 4 With CoO prepared by using water and ethanol as impregnating solution x /BiVO 4 XRD diffraction pattern of nanoplatelets.
FIG. 2 is a CoO prepared according to the present invention x /BiVO 4 SEM image of nanoplatelets.
FIG. 3 is a CoO prepared according to the present invention x /BiVO 4 XPS map of nanoplatelets.
FIG. 4 is a pure BiVO prepared according to the present invention 4 With CoO x /BiVO 4 UV-Vis DRS map and Tauc map of nanoplatelets.
FIG. 5 shows the pure BiVO prepared according to the present invention 4 With CoO x /BiVO 4 PL spectrum of nanoplatelets.
FIG. 6 is the present inventionCoO when the prepared impregnating solution is ethanol x /BiVO 4 SEM images of nanoplatelets and corresponding Mapping images.
FIG. 7 is a CoO of the impregnating solution prepared by the present invention in the case of water x /BiVO 4 SEM images of nanoplatelets and corresponding Mapping images.
FIG. 8 is a pure BiVO prepared according to the present invention 4 With CoO prepared by using water and ethanol as impregnating solution x /BiVO 4 Degradation profile of nanoplatelets degrading 50mL of 10mg/L BPA solution.
Detailed Description
The invention is further described below in connection with specific embodiments.
The terms such as "upper", "lower", "left", "right", "middle" and the like are also used in the present specification for convenience of description, and are not intended to limit the scope of the present invention, but rather to change or adjust the relative relationship thereof, and are also considered to be within the scope of the present invention without substantial change of technical content.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
As used herein, the term "about" is used to provide the flexibility and inaccuracy associated with a given term, metric or value. The degree of flexibility of a particular variable can be readily determined by one skilled in the art.
As used herein, the term "is intended to be synonymous with" one or more of ". For example, "at least one of A, B and C" expressly includes a only, B only, C only, and respective combinations thereof.
Concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of about 1 to about 4.5 should be interpreted to include not only the explicitly recited limits of 1 to about 4.5, but also include individual numbers (such as 2, 3, 4) and subranges (such as 1 to 3, 2 to 4, etc.). The same principle applies to ranges reciting only one numerical value, such as "less than about 4.5," which should be construed to include all such values and ranges. Moreover, such an interpretation should apply regardless of the breadth of the range or the characteristics being described.
Any steps recited in any method or process claims may be performed in any order and are not limited to the order set forth in the claims.
Example 1
The present embodiment provides a CoO x /BiVO 4 A method of preparing a nanoplatelet, the method comprising the steps of:
s1: 4mmol of Bi (NO) 3 ) 3 ·5H 2 O and 0.5g of SDBS were dissolved in 15mL of 4M HNO 3 Obtaining a solution A in the solution; 4mmol of NH 4 VO 3 Dissolving in 15mL of 2M NaOH solution to obtain solution B; dropwise adding the solution B into the solution A by using a peristaltic pump, wherein the rotating speed of the peristaltic pump is 80r/min; adjusting the pH value of the solution to 7, and uniformly stirring the solution by using a magnetic stirrer to obtain a precursor solution;
s2: carrying out hydrothermal reaction on the precursor liquid in the step S1 for 1h at 180 ℃ to obtain yellow precipitate, washing the yellow precipitate with water, washing with alcohol, and drying to obtain BiVO 4 ；
S3: biVO in 100mgS2 4 And 5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of ethanol, uniformly dispersing by ultrasonic waves, and drying; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 A nano-sheet.
The results are shown in FIG. 1-5, FIG. 1 shows the pure BiVO prepared according to the present invention 4 With CoO prepared by using water and ethanol as impregnating solution x /BiVO 4 XRD diffraction pattern of nano sheet, in which diffraction peak average is identical to monoclinic crystal phase BiVO 4 Corresponds to the standard card (PDF#14-0688), thus the BiVO prepared 4 In the monoclinic phase, coO is not visible in the figure x The reason for the diffraction peak of (2) is CoO x Low loading and high dispersibility of (3); FIG. 2 is CoO x /BiVO 4 SEM image of nanoplatelets; FIG. 3 is CoO x /BiVO 4 XPS image of nanoplatelets reveals BiVO 4 Is 2+ and 3+ in the presence of Co; FIG. 4 is pure BiVO 4 With CoO x /BiVO 4 UV-Vis DRS and Tauc images of nanoplatelets, demonstrating CoO x /BiVO 4 The utilization rate of the nano-sheet to visible light is higher than that of pure BiVO 4 And CoO x /BiVO 4 The band gap width (2.34 eV) of the nano-sheet is smaller than that of pure BiVO 4 (2.49 eV); FIG. 5 is pure BiVO 4 With CoO x /BiVO 4 PL spectra of nanoplatelets, demonstrating CoO between wavelengths 500nm and 900nm x /BiVO 4 The nano-sheets have better photogenerated carrier separation efficiency and stronger catalytic performance.
Comparative example 1
The present embodiment provides a CoO x /BiVO 4 The preparation method of the nano-sheet has the specific steps similar to those of the embodiment 1, wherein the difference is that water is selected as the impregnating solution in the step S3, namely,
s3: biVO in 100mgS2 4 And 5mg of Co (NO) 3 ) 2 ·6H 2 O is dissolved in 10mL of water, and is dried after being evenly dispersed by ultrasonic; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 A nano-sheet.
The results are shown in FIGS. 1, 6 and 7, and CoO is prepared by using water as the impregnating solution x /BiVO 4 Co in the nano-sheet is obviously agglomerated, and the dispersibility is better than that of CoO prepared by ethanol impregnating solution x /BiVO 4 The nanoplatelets are poor.
Example 2
The present embodiment provides a CoO x /BiVO 4 A method of preparing a nanoplatelet, the method comprising the steps of:
s1: 4mmol of Bi (NO) 3 ) 3 ·5H 2 O and 1.0g of SDBS were dissolved in 15mL of 4M HNO 3 Obtaining a solution A in the solution; 4mmol of NH 4 VO 3 Dissolving in 15mL of 2M NaOH solution to obtain solution B; dropwise adding the solution B into the solution A by using a peristaltic pump, wherein the rotating speed of the peristaltic pump is 70r/min; adjusting the pH value of the solution to 6.5, and uniformly stirring the solution by using a magnetic stirrer to obtain a precursor solution;
s2: carrying out hydrothermal reaction on the precursor liquid in the step S1 at 200 ℃ for 50min to obtain yellow precipitate, washing the yellow precipitate with water, washing with alcohol, and drying to obtain BiVO 4 ；
S3: 100mg of BiVO in S2 4 And 5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of ethanol, uniformly dispersing by ultrasonic waves, and drying; calcining the dried sample in a muffle furnace at 180 ℃ for 1.2h to obtain CoO x /BiVO 4 A nano-sheet.
The detection result shows CoO x /BiVO 4 The nano-sheet is prepared successfully.
Example 3
The present embodiment provides a CoO x /BiVO 4 A method of preparing a nanoplatelet, the method comprising the steps of:
s1: 5mmol of Bi (NO) 3 ) 3 ·5H 2 O and 1.875g of SDBS were dissolved in 15mL of 4M HNO 3 Obtaining a solution A in the solution; 5mmol of NH 4 VO 3 Dissolving in 15mL of 2M NaOH solution to obtain solution B; dropwise adding the solution B into the solution A by using a peristaltic pump, wherein the rotating speed of the peristaltic pump is 90r/min; adjusting the pH value of the solution to 6, and uniformly stirring the solution by using a magnetic stirrer to obtain a precursor solution;
s2: and (3) carrying out hydrothermal reaction on the precursor liquid in the step S1 at 160 ℃ for 70min to obtain yellow precipitate. Washing the yellow precipitate with water, washing with alcohol, and oven drying to obtain BiVO 4 ；
S3: 50mg of BiVO in S2 4 And 2.5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of ethanol, uniformly dispersing by ultrasonic waves, and drying; will beCalcining the dried sample in a muffle furnace at 220 ℃ for 0.8h to obtain CoO x /BiVO 4 A nano-sheet.
The detection result shows CoO x /BiVO 4 The nano-sheet is prepared successfully.
Example 4
The present embodiment provides a CoO x /BiVO 4 A method of preparing a nanoplatelet, the method comprising the steps of:
s1: 3mmol of Bi (NO) 3 ) 3 ·5H 2 O and 0.375g of SDBS were dissolved in 15mL of 4M HNO 3 Obtaining a solution A in the solution; 3mmol of NH 4 VO 3 Dissolving in 15mL of 2M NaOH solution to obtain solution B; dropwise adding the solution B into the solution A by using a peristaltic pump, wherein the rotating speed of the peristaltic pump is 80r/min; adjusting the pH value of the solution to 6.5, and uniformly stirring the solution by using a magnetic stirrer to obtain a precursor solution;
s2: and (3) carrying out hydrothermal reaction on the precursor liquid in the step S1 at 180 ℃ for 1h to obtain yellow precipitate. Washing the yellow precipitate with water, washing with alcohol, and oven drying to obtain BiVO 4 ；
S3: 150mg of BiVO in S2 4 And 7.5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of ethanol, uniformly dispersing by ultrasonic waves, and drying; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 A nano-sheet.
The detection result shows CoO x /BiVO 4 The nano-sheet is prepared successfully.
Example 5
This embodiment provides a CoO as in embodiment 1 above x /BiVO 4 The application of the nano-sheet is used for degrading BPA solution. The method specifically comprises the following steps:
s1: 40mg of the photocatalyst prepared in example 1 was added to 50mL of 10ppm BPA solution and sonicated for 3min;
s2: stirring the solution under dark condition for 30min;
s3: the solution was placed under a 500W xenon lamp for photocatalytic degradation. 1mL of sample is extracted every 1h in the reaction process, and the sample is filtered by a water phase filter head with the diameter of 0.22 mu m;
s4: and (3) measuring the concentration of BPA in the solution by adopting a high performance liquid chromatograph, and drawing a reaction curve.
As a result, as shown in FIG. 8, coO was prepared using ethanol as the impregnating solution x /BiVO 4 The degradation effect of the nano-sheet is obviously better than that of pure BiVO 4 With CoO prepared by selecting water as impregnating solution x /BiVO 4 The degradation effect of the nano-sheet.

Claims (7)

1. CoO (CoO) x /BiVO 4 The preparation method of the nano-sheet is characterized by comprising the following steps:
s1: bi (NO) 3 ) 3 ·5H 2 O and SDBS (sodium dodecyl benzene sulfonate) are dissolved in HNO 3 Obtaining a solution A in the solution; NH is added to 4 VO 3 Dissolving in NaOH solution to obtain solution B; dropwise adding the solution B into the solution A, adjusting the pH of the solution to 6-7, and uniformly stirring to obtain a precursor solution; bi (NO) in the solution A in S1 3 ) 3 ·5H 2 O and NH in solution B 4 VO 3 The molar concentrations are the same; bi (NO) in the solution A in S1 3 ) 3 ·5H 2 The molar concentration of O is 0.2-0.34 mmol/mL;
s2: carrying out hydrothermal reaction on the precursor liquid in the step S1 at 160-200 ℃ for 50-70 min to obtain yellow precipitate; washing the yellow precipitate with water, washing with alcohol, and oven drying to obtain BiVO 4 ；
S3: biVO in S2 4 And Co (NO) 3 ) 2 ·6H 2 Dissolving O in ethanol, uniformly dispersing by ultrasonic waves, and drying; calcining the dried sample in a muffle furnace at 180-220 ℃ for 0.8-2.0 h to obtain CoO x /BiVO 4 A nanosheet; ethanol relative to 1mL in S3, biVO 4 The dosage of the catalyst is 5-15 mg, co (NO) 3 ) 2 ·6H 2 The dosage of O is 0.25-0.75 mg.
2. The CoO of claim 1 x /BiVO 4 A method for producing a nanosheet, characterized in that the nanosheet is produced from 1mmol Bi (NO 3 ) 3 ·5H 2 The amount of O and SDBS is 0.125-0.375 g.
3. The CoO of claim 2 x /BiVO 4 The preparation method of the nano-sheet is characterized in that a peristaltic pump is used for dropwise adding the solution B into the solution A in the step S1, and the rotation speed of the peristaltic pump is 70-90 r/min.
4. The CoO of claim 3 x /BiVO 4 The preparation method of the nano-sheet is characterized in that the hydrothermal reaction temperature in S2 is 180 ℃ and the reaction time is 1h.
5. The CoO of claim 4 x /BiVO 4 The preparation method of the nano-sheet is characterized in that the calcination temperature in S3 is 200 ℃ and the time is 2.0 h.
6. CoO (CoO) x /BiVO 4 The nano-sheet is characterized by being prepared by the preparation method of any one of claims 1-5.
7. The CoO of claim 6 x /BiVO 4 The application of the nano-sheet is characterized in that CoO x /BiVO 4 The nanosheets are used for photoelectrocatalysis.
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CN105964277A (en) * 2016-05-13 2016-09-28 南京理工大学 CdS/BiVO4 composite photocatalyst and preparation method thereof
CN107096523A (en) * 2017-05-17 2017-08-29 重庆大学 A kind of knitting wool ball composite photo-catalyst carbon doping pucherite@multi-walled carbon nanotubes and preparation method thereof
CN113896243A (en) * 2021-09-29 2022-01-07 陕西科技大学 BiVO4Nanosheet and preparation method and application thereof

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CN105964277A (en) * 2016-05-13 2016-09-28 南京理工大学 CdS/BiVO4 composite photocatalyst and preparation method thereof
CN107096523A (en) * 2017-05-17 2017-08-29 重庆大学 A kind of knitting wool ball composite photo-catalyst carbon doping pucherite@multi-walled carbon nanotubes and preparation method thereof
CN113896243A (en) * 2021-09-29 2022-01-07 陕西科技大学 BiVO4Nanosheet and preparation method and application thereof

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