CN115025784A - CoOx/BiVO 4 Nanosheet and preparation method and application thereof - Google Patents

CoOx/BiVO 4 Nanosheet and preparation method and application thereof Download PDF

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CN115025784A
CN115025784A CN202210679053.5A CN202210679053A CN115025784A CN 115025784 A CN115025784 A CN 115025784A CN 202210679053 A CN202210679053 A CN 202210679053A CN 115025784 A CN115025784 A CN 115025784A
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bivo
solution
coo
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nanosheet
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CN115025784B (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 CoOx/BiVO 4 Nanosheet and a preparation method and application thereof, belonging to the field of semiconductor materials. The method prepares BiVO through hydrothermal reaction 4 During the preparation, the low temperature (1111111 ℃) and the short reaction time (51171min) are used, so that the preparation time is shortened, a good nano flaky shape 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; at the same timeThe method selects absolute ethyl alcohol as the immersion liquid, shortens the drying time, enables the composite material to obtain narrower band gap width, improves the visible light utilization capacity of the composite material, and enables the separation effect of photon-generated carriers of the composite material to be better.

Description

CoOx/BiVO 4 Nanosheet and preparation method and application thereof
Technical Field
The invention belongs to the field of semiconductor materials, and particularly relates to a CoO x /BiVO 4 Nanosheet and preparation method and application thereof.
Background
BiVO 4 The material is a common n-type semiconductor photocatalytic material and mainly has three crystal structures: tetragonal scheelite type, tetragonal zircon type and monoclinic scheelite type. Wherein, 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 narrow, so that the recombination probability of a photon-generated carrier is high, and the photocatalytic performance needs to be further improved.
In order to increase BiVO 4 The photocatalysis performance is controlled by methods of morphology regulation, semiconductor compounding and the like commonly used in the prior art for BiVO 4 And (4) carrying out modification. In improving BiVO 4 Among various methods of photocatalytic performance, constructing a p-n heterostructure is considered to be the most effective method for improving the activity of a photocatalyst. CoO x As an important p-type semiconductor material, the p-type semiconductor material has low cost, no toxicity, good stability and the likeHas the advantages of good application prospect in the field of photocatalysis. Due to CoO x And BiVO 4 Band structure matching, CoO x Can be reacted with BiVO 4 Forming p-n heterostructure to make photo-generated electrons in BiVO 4 Surface enrichment of photogenerated holes in CoO x The surface enrichment improves the carrier separation rate, thereby improving the photocatalytic performance.
The Chinese patent with the publication number of CN109794256A discloses a preparation method and an application of a bismuth vanadate composite material loaded with cobalt oxide nanoparticles, which is to mix BiVO 4 Soaking the film in CoCl 2 Adding Co into the solution for 10-12 h 2+ The adsorption balance is achieved; then will absorb Co 2+ BiVO (b) 4 The film is placed in a drying oven for drying, then placed in a muffle furnace, and calcined for 4-5 hours at the high temperature of 450-500 ℃ to obtain the loaded CoO x BiVO (b) 4 Thin film CoO x /BiVO 4 . The preparation time is about 14-17 h, and the high-temperature calcination at 450-500 ℃ is required. The calcination is carried out for a longer time and at a higher temperature, the energy consumption is higher, the preparation cost of the catalyst is increased, and BiVO (bismuth vanadium oxide) can be caused 4 Agglomeration occurs, destroying the structure itself, resulting in a decrease in photocatalytic performance.
This patent discloses a CoO x /BiVO 4 The composite material prepared by the method has a narrow band gap and good visible light utilization performance, photogenerated carriers can be effectively separated, and BiVO (BiVO) is effectively improved 4 The photocatalytic performance of (a).
Disclosure of Invention
1. Problems to be solved
The invention aims at the CoO in the prior art x /BiVO 4 The problems of high energy consumption and insufficient catalytic performance of the final product caused by long preparation time and high temperature in the preparation process of the catalyst are solved, and the CoO is provided x /BiVO 4 Nanosheet and preparation method and application thereof.
2. Technical scheme
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 nanoplatelets, the method comprising the steps of:
s1: adding Bi (NO) 3 ) 3 ·5H 2 O and SDBS (sodium dodecyl benzene sulfonate) dissolved in HNO 3 Obtaining a solution A in the solution; reacting NH 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;
s2: carrying out hydrothermal reaction on the precursor solution in the S1 at 160-200 ℃ for 50-70 min to obtain yellow precipitate; washing the yellow precipitate with water, washing with alcohol, and drying to obtain BiVO 4 ；
S3: BiVO in S2 4 And Co (NO) 3 ) 2 ·6H 2 Dissolving O in ethanol, ultrasonically dispersing uniformly, 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 Nanosheets.
Preferably, Bi (NO) is contained in the solution A in S1 3 ) 3 ·5H 2 O and NH in solution B 4 VO 3 The molar concentrations were the same.
Preferably, Bi (NO) is contained in the solution A in S1 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 0.27 mmol/mL.
Preferably, the above-mentioned S1 is performed with respect to 1mmol of Bi (NO) 3 ) 3 ·5H 2 The dosage of the O and the SDBS is 0.125-0.375 g. Further, SDBS was used in an amount of 0.25 g.
Preferably, the HNO of 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. Furthermore, the speed of the peristaltic pump is 80 r/min.
Preferably, the stirring in S1 is performed by using a magnetic stirrer.
Preferably, the hydrothermal reaction temperature in the above S2 is 180 ℃ and the reaction time is 1 h.
Preference is given toBiVO relative to 1mL of ethanol in S3 4 The amount of Co (NO) is 5-15 mg 3 ) 2 ·6H 2 The dosage of O is 0.25-0.75 mg. Further, BiVO 4 In an amount of 10mg, Co (NO) 3 ) 2 ·6H 2 The amount of O is 0.25 mg.
Preferably, the calcination temperature in the S3 is 200 ℃ and the calcination time is 2 h.
The invention also provides a CoO x /BiVO 4 A nanosheet prepared by the above-described preparation method.
The invention also provides the CoO x /BiVO 4 Use of nanosheets or of a method of preparation of CoO x /BiVO 4 The nanosheets are useful 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 Preparation method of nanosheet, and BiVO prepared by hydrothermal reaction 4 In the process, the low temperature (160-200 ℃) and the short reaction time (50-70 min) are used, so that the preparation time is shortened, and the good nano flaky morphology can be formed at the same time, because the BiVO in the solution can be possibly caused by the high hydrothermal temperature and the long reaction time 4 Ostwald curing occurs, and the Ostwald is agglomerated to form a blocky structure, while the nano flaky shape can obviously increase the specific surface area of the catalyst and provide more adsorption sites and active sites, thereby improving the photocatalytic performance.
(2) The invention provides a CoO x /BiVO 4 The preparation method of the nanosheet selects the absolute ethyl alcohol as the impregnation liquid, shortens the drying time, enables the composite material to obtain a narrower band gap width, improves the visible light utilization capacity of the composite material, and enables the separation effect of the photon-generated carriers of the composite material to be better. As can be seen from FIG. 1, CoO was prepared by using ethanol as the immersion liquid x /BiVO 4 The diffraction peak intensity of the nanosheet is higher than that of CoO prepared by using water as impregnation liquid x /BiVO 4 The nanoplatelets are weaker and presumably areBecause ethanol is used as the impregnation liquid to improve CoOx in BiVO 4 Dispersion of (2). Thus, the CoO prepared using ethanol as the impregnating solution x /BiVO 4 The nano-sheet has better photocatalysis effect.
Drawings
FIG. 1 is pure BiVO prepared by the present invention 4 CoO prepared by using water and ethanol as impregnation liquid x /BiVO 4 XRD diffraction pattern of the nano-sheet.
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 images of nanoplatelets.
FIG. 4 is a pure BiVO prepared by the present invention 4 With CoO x /BiVO 4 UV-Vis DRS diagram and Tauc diagram of the nano-sheet.
FIG. 5 is pure BiVO prepared by the present invention 4 And CoO x /BiVO 4 PL spectrum of the nanoplate.
FIG. 6 shows CoO when ethanol is used as the dipping solution prepared by the present invention x /BiVO 4 SEM images and corresponding Mapping images of the nanoplatelets.
FIG. 7 is a CoO of water as the immersion fluid prepared in the present invention x /BiVO 4 SEM images and corresponding Mapping images of the nanoplatelets.
FIG. 8 is pure BiVO prepared by the present invention 4 CoO prepared by using water and ethanol as impregnation liquid x /BiVO 4 Degradation profile of 50mL of 10mg/L BPA solution degraded by the nanoplatelets.
Detailed Description
The invention is further described with reference to specific examples.
It should be noted that the terms "upper", "lower", "left", "right" and "middle" used in the present specification are for the sake of clarity, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof may be made without substantial technical changes.
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; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
As used herein, the term "about" is used to provide the flexibility and inaccuracy associated with a given term, measure or value. The degree of flexibility for a particular variable can be readily determined by one skilled in the art.
As used herein, at least one of the terms "is intended to be synonymous with one or more of. For example, "at least one of A, B and C" explicitly includes a only, B only, C only, and combinations thereof, respectively.
Concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such a 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 limit values of 1 to about 4.5, but also include individual numbers (such as 2, 3, 4) and sub-ranges (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 of the aforementioned values and ranges. Further, such 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 executed in any order and are not limited to the order presented in the claims.
Example 1
This example provides a CoO x /BiVO 4 A method of preparing nanoplatelets, the method comprising the steps of:
s1: 4mmol of Bi (NO) 3 ) 3 ·5H 2 O and 0.5g SDBS in 15mL 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 80 r/min; adjusting the pH value of the solution to 7, and uniformly stirring the solution by using a magnetic stirrer to obtain precursor solution;
s2: carrying out hydrothermal reaction on the precursor solution in S1 at 180 ℃ for 1h 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, performing ultrasonic dispersion uniformly, and drying; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 Nanosheets.
The results are shown in FIGS. 1-5, where FIG. 1 is pure BiVO prepared according to the invention 4 CoO prepared by using water and ethanol as impregnation liquid x /BiVO 4 The XRD diffraction pattern of the nano-sheet has diffraction peaks which are all matched with monoclinic phase BiVO 4 Corresponds to the standard card (PDF #14-0688), thus preparing BiVO 4 The monoclinic phase, no CoO is visible x The reason for the diffraction peak of (2) is CoO x Low loading and high dispersion; FIG. 2 is CoO x /BiVO 4 SEM images of the nanoplatelets; FIG. 3 is CoO x /BiVO 4 XPS plot of nanoplates revealing BiVO 4 The existing valence states of Co are 2+ and 3 +; FIG. 4 is pure BiVO 4 With CoO x /BiVO 4 The UV-Vis DRS diagram and Tauc diagram of the nano sheet prove CoO x /BiVO 4 The utilization rate of the nano-sheets to visible light is higher than that of pure BiVO 4 And CoO x /BiVO 4 The band gap width (2.34eV) of the nanosheets is less than that of pure BiVO 4 (2.49 eV); FIG. 5 is pure BiVO 4 With CoO x /BiVO 4 PL spectrogram of the nano-sheet proves that CoO is between 500nm and 900nm in wavelength x /BiVO 4 The nano-sheets have better photon-generated carrier separation efficiency and stronger catalytic performance.
Comparative example 1
This example provides a CoO x /BiVO 4 The preparation method of the nanosheet is the same as that of example 1, except that water is selected as the impregnating solution in S3, i.e.,
s3: 100mgS2 of BiVO 4 And 5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of water, uniformly dispersing by ultrasonic, and drying; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 Nanosheets.
As a result, CoO was produced using water as the immersion liquid as shown in FIGS. 1, 6 and 7 x /BiVO 4 Co in the nanosheets is obviously agglomerated, and the dispersity of the Co is higher than that of CoO prepared from ethanol impregnation liquid x /BiVO 4 The nanoplatelets are poor.
Example 2
This example provides a CoO x /BiVO 4 A method of preparing nanoplatelets, the method comprising the steps of:
s1: 4mmol of Bi (NO) 3 ) 3 ·5H 2 O and 1.0g of SDBS 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 70 r/min; adjusting the pH value of the solution to 6.5, and uniformly stirring the solution by using a magnetic stirrer to obtain precursor solution;
s2: carrying out hydrothermal reaction on the precursor solution in the 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, performing ultrasonic dispersion uniformly, and drying; calcining the dried sample in a muffle furnace at 180 ℃ for 1.2h to obtain CoO x /BiVO 4 Nanosheets.
The detection result shows CoO x /BiVO 4 Nano-sheetThe preparation is successful.
Example 3
This example provides a CoO x /BiVO 4 A method of preparing nanoplatelets, the method comprising the steps of:
s1: adding 5mmol of Bi (NO) 3 ) 3 ·5H 2 O and 1.875g of SDBS in 15mL of 4M HNO 3 Obtaining a solution A in the solution; adding 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 90 r/min; adjusting the pH value of the solution to 6, and uniformly stirring the solution by using a magnetic stirrer to obtain precursor solution;
s2: and carrying out hydrothermal reaction on the precursor solution in the S1 at 160 ℃ for 70min to obtain yellow precipitate. Washing the yellow precipitate with water, washing with alcohol, and 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, performing ultrasonic dispersion uniformly, and drying; calcining the dried sample in a muffle furnace at 220 ℃ for 0.8h to obtain CoO x /BiVO 4 Nanosheets.
The detection result shows CoO x /BiVO 4 The preparation of the nano-sheet is successful.
Example 4
The present embodiment provides a CoO x /BiVO 4 A method of preparing nanoplatelets, the method comprising the steps of:
s1: 3mmol of Bi (NO) 3 ) 3 ·5H 2 O and 0.375g SDBS in 15mL 4M HNO 3 Obtaining a solution A in the solution; adding 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 80 r/min; adjusting the pH value of the solution to 6.5, and uniformly stirring the solution by using a magnetic stirrer to obtain precursor solution;
s2: and carrying out hydrothermal reaction on the precursor solution in the S1 at 180 ℃ for 1h to obtain yellow precipitate. Washing the yellow precipitate with water, washing with alcohol, and drying to obtain BiVO 4 ；
S3: 150mg of Bi in S2VO 4 And 7.5mg of Co (NO) 3 ) 2 ·6H 2 Dissolving O in 10mL of ethanol, performing ultrasonic dispersion uniformly, and drying; calcining the dried sample in a muffle furnace at 200 ℃ for 2h to obtain CoO x /BiVO 4 Nanosheets.
The detection result shows CoO x /BiVO 4 The nano-sheet is successfully prepared.
Example 5
This example provides a CoO as in example 1 above x /BiVO 4 Use of nanoplatelets for degrading a BPA solution. The method specifically comprises the following steps:
s1: adding 40mg of the photocatalyst prepared in example 1 into 50mL of 10ppm BPA solution, and carrying out ultrasonic treatment for 3 min;
s2: stirring the solution for 30min under dark condition;
s3: the solution was placed under a 500W xenon lamp for photocatalytic degradation. During the reaction, 1mL of sample is extracted every 1h and filtered by a 0.22 mu m aqueous phase filter head;
s4: and (4) measuring the concentration of the BPA in the solution by using a high performance liquid chromatograph, and drawing a reaction curve.
The results are shown in FIG. 8, CoO prepared with ethanol as the immersion liquid x /BiVO 4 The degradation effect of the nano-sheets is obviously better than that of pure BiVO 4 With CoO prepared by using water as impregnating solution x /BiVO 4 And (3) degradation effect of the nanosheets.

Claims (10)

1. CoO (cobalt oxide) x /BiVO 4 The preparation method of the nanosheet is characterized by comprising the following steps:
s1: adding Bi (NO) 3 ) 3 ·5H 2 O and SDBS (sodium dodecyl benzene sulfonate) dissolved in HNO 3 Obtaining a solution A in the solution; reacting NH 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;
s2: carrying out hydrothermal reaction on the precursor solution in the S1 at 160-200 ℃ for 50-70 min to obtain yellow precipitate; washing the yellow precipitate with water, washing with alcohol, and drying to obtain BiVO 4 ；
S3: BiVO in S2 4 And Co (NO) 3 ) 2 ·6H 2 Dissolving O in ethanol, ultrasonically dispersing uniformly, 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.
2. The CoO of claim 1 x /BiVO 4 A process for the preparation of nanoplatelets characterized in that in S1, Bi (NO) is present in solution A 3 ) 3 ·5H 2 O and NH in solution B 4 VO 3 The molar concentrations were the same.
3. The CoO of claim 2 x /BiVO 4 The preparation method of the nano-sheet is characterized in that Bi (NO) in solution A in S1 3 ) 3 ·5H 2 The molar concentration of O is 0.2-0.34 mmol/mL.
4. The CoO of claim 3 x /BiVO 4 A process for producing nanosheets, wherein S1 is defined as being 1mmol of Bi (NO) 3 ) 3 ·5H 2 The dosage of the O and the SDBS is 0.125-0.375 g.
5. The CoO of claim 4 x /BiVO 4 The preparation method of the nanosheet is characterized in that in S1, the solution B is dropwise added into the solution A by using a peristaltic pump, and the rotating speed of the peristaltic pump is 70-90 r/min.
6. CoO according to claim 4 or 5 x /BiVO 4 A method for producing a nanosheet, wherein BiVO is present in S3 in an amount of 1mL of ethanol 4 The dosage of (A) is 5-15 mg, Co (NO) 3 ) 2 ·6H 2 The dosage of O is 0.25-0.75 mg.
7. The CoO of claim 6 x /BiVO 4 A process for the preparation of nanoplatelets characterized in thatThe hydrothermal reaction temperature in the S2 is 180 ℃, and the reaction time is 1 h.
8. CoO according to claim 6 or 7 x /BiVO 4 The preparation method of the nanosheet is characterized in that the calcining temperature in S3 is 200 ℃ and the time is 2.0 h.
9. CoO (cobalt oxide) x /BiVO 4 Nanosheet, characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. The process according to any of claims 1 to 8 and/or the CoO according to claim 9 x /BiVO 4 Use of nanosheets, characterised in that CoO is added x /BiVO 4 The nanosheets are useful 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
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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
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CN115947383A (en) * 2022-12-28 2023-04-11 青岛科技大学 Cobalt oxide-loaded bismuth vanadate nanosheet piezoelectric catalyst and preparation method and application thereof

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