CN113457698B - Method for improving BiOCl surface photovoltage signal - Google Patents
Method for improving BiOCl surface photovoltage signal Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 107
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229960000583 acetic acid Drugs 0.000 claims abstract description 37
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 37
- 239000000725 suspension Substances 0.000 claims abstract description 35
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 18
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001291 vacuum drying Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 23
- 238000002360 preparation method Methods 0.000 description 13
- 238000009210 therapy by ultrasound Methods 0.000 description 11
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 230000003313 weakening effect Effects 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the field of material chemistry, in particular to the field of photocatalytic materials, and specifically relates to a method for improving a BiOCl surface photovoltage signal. The method comprises the following steps: dispersing black phosphorus powder in glacial acetic acid with a certain volume, and performing ultrasonic dispersion; bismuth nitrate was added to dissolve in the black phosphorus-glacial acetic acid suspension, and a KCl solution (the number of moles of KCl is equal to the number of moles of bismuth nitrate) was added dropwise to the bismuth nitrate-glacial acetic acid-black phosphorus suspension. Transferring the generated suspension system into a hydrothermal reaction kettle for hydrothermal reaction, naturally cooling the hydrothermal reaction to room temperature, washing the precipitate with deionized water and alcohol, taking out, and vacuum drying to obtain a sample. The surface photovoltage signal of the BiOCl sample prepared by assisting with a proper amount of black phosphorus is obviously enhanced in the range of 300-400 nm. The invention has simple operation, easy realization, safety and reliability.
Description
Technical Field
The invention relates to the field of material chemistry, in particular to the field of photocatalytic materials, and specifically relates to a method for improving a BiOCl surface photovoltage signal.
Background
BiOCl is a ternary oxide composed of V-VI-VII main group elements, the crystal structure belongs to a PbFCl layered structure, has high anisotropy and wide forbidden band width of 3.0-3.5 eV, and has a special layered structure and proper forbidden band width, so that the BiOCl is one of excellent photocatalytic materials. Electrons on the valence band of the BiOCl photocatalyst under excitation of light of sufficient energy (e - ) Absorbs enough energy to transit across the forbidden band to the conduction band, leaving a photogenerated void in the valence band (h + ) Thus, a photogenerated electron-hole pair (e - -h + ). Electrons migrating to the surface of BiOCl and organic matters adsorbed on the surfaceThe living reactions and the holes are oxidized with the organic matters adsorbed on the surface.
The composite reaction between the photo-generated electrons and the holes can release energy in the form of light or heat, so that the photocatalytic performance of the photocatalyst is greatly reduced. Therefore, the photocatalytic efficiency of the BiOCl is mainly affected by the frequency and intensity of the incident light, the forbidden bandwidth of the photocatalyst, and the recombination rate of the photo-generated electrons and holes.
The photocatalytic reaction occurs on the surface of the photocatalyst, and the photocatalytic surface property can significantly influence the photogenerated charge separation efficiency, thereby influencing the photocatalytic activity. It follows that surface modification is an effective means of increasing the photo-catalytic activity of BiOCl. However, at present, no better method for surface modification exists.
Disclosure of Invention
The invention aims to solve the problems and provide a method for improving the BiOCl surface photovoltage signal, which is assisted by black phosphorus and can enhance the BiOCl surface photovoltage signal by proper amount of black phosphorus surface modification; the black phosphorus surface modification can influence the growth of BiOCl, build defects, capture photo-generated electrons, inhibit the recombination of the photo-generated electrons and holes, and obtain the BiOCl with enhanced surface photovoltage signals.
In order to achieve the above object, the present invention has the following specific technical scheme:
a method of increasing a BiOCl surface photovoltage signal comprising the steps of:
1) Dispersing a proper amount of black phosphorus into glacial acetic acid to obtain a black phosphorus-glacial acetic acid suspension system; and then bismuth nitrate is dissolved in a black phosphorus-glacial acetic acid suspension system to obtain bismuth nitrate-glacial acetic acid-black phosphorus suspension.
2) Dropwise adding KCl solution into bismuth nitrate-glacial acetic acid-black phosphorus suspension, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction, and naturally cooling to room temperature.
3) Washing the sample with deionized water, washing with alcohol, and vacuum drying.
As a preferred embodiment in the present application, the black phosphorus is orthorhombic black phosphorus.
As a preferred embodiment in the application, the ratio of the adding amount g of bismuth nitrate to the volume mL of glacial acetic acid is 1:8-12.
As a preferred embodiment in the present application, the mass ratio of black phosphorus to BiOCl produced is 0.1% -1.9%.
As a preferred embodiment in the present application, the hydrothermal reaction temperature is 140-180 ℃ and the time is 12-24 hours.
As a preferred embodiment in the present application, the number of alcohol washes is 1-2.
As a preferred embodiment in the present application, the temperature of the vacuum drying is 60.+ -. 5 ℃.
The BiOCl prepared by the method has obviously enhanced surface photovoltage signal in the range of 300-400 nm.
The principle of the application is as follows: black phosphorus is a solid having metallic luster, has a wavy layered structure, and has weaker bonding between layers than bonding between layers, and has conductivity. The application uses a proper amount of black phosphorus to modify the surface of BiOCl to construct defects, and simultaneously utilizes the conductivity of the black phosphorus to improve the separation of photo-generated charges and display higher surface photovoltage signals.
Compared with the prior art, the invention has the following beneficial effects:
the processing method of the surface photovoltage signal obviously enhanced BiOCl is simple and convenient to operate, easy to realize, safe and reliable.
And secondly, the BiOCl obtained by surface modification of a proper amount of black phosphorus has obviously enhanced surface photovoltage signals in a range of 300-400nm, which has important practical significance for improving the photocatalytic activity.
Drawings
FIG. 1 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus and the samples obtained in example 1.
FIG. 2 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus and the samples obtained in example 2.
FIG. 3 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus and the samples obtained in example 3.
FIG. 4 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus and the samples obtained in example 4.
FIG. 5 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus and the samples obtained in example 5.
FIG. 6 is a comparison of surface photovoltage signals for BiOCl prepared without black phosphorus and the samples obtained in example 6.
FIG. 7 is a comparison of surface photovoltage signals for BiOCl prepared without black phosphorus and the samples obtained in example 7.
FIG. 8 is a comparison of surface photovoltage signals for BiOCl prepared without black phosphorus and samples obtained in example 8.
FIG. 9 is a surface photovoltage signal comparison of BiOCl prepared without red phosphorus and the sample obtained in example 9.
FIG. 10 is a comparison of the surface photovoltage signals of BiOCl prepared without red phosphorus and the samples obtained in example 10.
FIG. 11 is a surface photovoltage signal comparison of BiOCl prepared without red phosphorus and the sample obtained in example 11.
Detailed Description
A method of increasing a BiOCl surface photovoltage signal comprising the steps of:
the first step: dispersing a proper amount of black phosphorus into glacial acetic acid, and dissolving bismuth nitrate into a black phosphorus-glacial acetic acid suspension system; preferably, bismuth nitrate/glacial acetic acid volume: the mass ratio of the black phosphorus to the BiOCl is 0.1-1.9% from 5g/40mL to 5g/60 mL.
And a second step of: dropwise adding KCl solution into bismuth nitrate-glacial acetic acid-black phosphorus suspension, transferring the generated precipitate into a hydrothermal reaction kettle, performing hydrothermal treatment at 140-180 ℃ for 12-24 hours, and naturally cooling to room temperature.
And a third step of: washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at about 60deg.C to obtain the final product.
Preferably, the black phosphorus is orthorhombic black phosphorus; the mass ratio of the black phosphorus to the BiOCl is 0.1-1.9%.
The BiOCl prepared by the method has obviously enhanced surface photovoltage signal in the range of 300-400nm
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In the following examples, the surface photovoltage test is carried out on a surface photovoltage spectrum assembled by Jilin university, the light source is a xenon lamp, the collected signals are amplified by adopting a lock-in amplifier, the sample is pressed between conductive glass and a metal copper base, the wavelength test range is 300-400nm, and the specific test method and operation adopt conventional technical means.
Comparative example 1
1) 5g bismuth nitrate was dissolved in 40mL glacial acetic acid; to the bismuth nitrate-glacial acetic acid solution was added dropwise 10mL of a solution of KCl, the moles of KCl being equal to the moles of bismuth nitrate. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 24 hours at 180 ℃, and naturally cooling to room temperature.
2) Filtering, washing with deionized water, washing with alcohol for 1-2 times, vacuum drying at 60deg.C, taking out the obtained solid, grinding, and testing photovoltage signal.
Example 1
The preparation process of the surface photovoltage signal enhancement type BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 40mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 0.1%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a black phosphorus/BiOCl mass ratio of 0.1%.
FIG. 1 is a graph showing comparison of surface photovoltage signals of samples obtained in example 1 and comparative example 1. As can be seen from FIG. 1, the BiOCl prepared by the assistance of black phosphorus has significantly enhanced surface photovoltage signal in the range of 300-400nm compared with BiOCl prepared without the assistance of black phosphorus, and the BiOCl surface photovoltage signal can be enhanced by the assistance of black phosphorus.
Example 2
The specific preparation process of the surface photovoltage signal enhancement type BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 50mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 0.5%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 140 ℃ for 12 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a black phosphorus/generated BiOCl mass ratio of 0.5% and a hydrothermal temperature of 140 ℃ and a hydrothermal time of 12 hours.
FIG. 2 is a graph showing comparison of surface photovoltage signals of samples obtained in example 2 and comparative example 1. As can be seen from fig. 2, the surface photovoltage signal of the BiOCl prepared with the assistance of black phosphorus is significantly enhanced in the range of 300-400nm compared with that of the BiOCl prepared without the assistance of black phosphorus, and the surface photovoltage signal of the BiOCl can be enhanced by the assistance of black phosphorus.
Example 3
The specific preparation process of the surface photovoltage signal enhancement type BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 60mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 1%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 18 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a mass ratio of 1% to the resultant BiOCl, a hydrothermal temperature of 160℃and a hydrothermal time of 18 hours.
FIG. 3 is a graph showing comparison of surface photovoltage signals of samples obtained in example 3 and comparative example 1. As can be seen from fig. 3, the surface photovoltage signal of the BiOCl prepared with the assistance of black phosphorus is significantly enhanced in the range of 300-400nm compared with that of the BiOCl prepared without the assistance of black phosphorus, and the surface photovoltage signal of the BiOCl can be enhanced by the assistance of black phosphorus.
Example 4
The specific preparation process of the surface photovoltage signal enhancement type BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 45mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 1.5%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 12 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a mass ratio of 1.5% to the resultant BiOCl, a hydrothermal temperature of 180℃and a hydrothermal time of 12 hours.
FIG. 4 is a graph showing comparison of surface photovoltage signals of samples obtained in example 4 and comparative example 1. As can be seen from fig. 4, the surface photovoltage signal of the BiOCl prepared with the assistance of black phosphorus is significantly enhanced in the range of 300-400nm compared with that of the BiOCl prepared without the assistance of black phosphorus, and the surface photovoltage signal of the BiOCl can be enhanced by the assistance of black phosphorus.
Example 5
The specific preparation process of the surface photovoltage signal enhancement type BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 45mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 1.9%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 20 hours at 140 ℃, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a mass ratio of 1.9% to the resultant BiOCl, a hydrothermal temperature of 140℃and a hydrothermal time of 20 hours.
FIG. 5 is a graph showing comparison of surface photovoltage signals of samples obtained in example 5 and comparative example 1. As can be seen from fig. 5, the surface photovoltage signal of the BiOCl prepared with the assistance of black phosphorus is significantly enhanced in the range of 300-400nm compared with that of the BiOCl prepared without the assistance of black phosphorus, and the surface photovoltage signal of the BiOCl can be enhanced by the assistance of black phosphorus.
Example 6
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 55mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 2%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In contrast to comparative example 1, black phosphorus was added at a black phosphorus/BiOCl mass ratio of 2%, a hydrothermal temperature of 140 ℃ and a hydrothermal time of 20h.
FIG. 6 is a graph showing comparison of surface photovoltage signals of samples obtained in example 6 and comparative example 1. As can be seen from FIG. 6, the BiOCl prepared with the assistance of black phosphorus has a reduced surface photovoltage signal in the range of 300-400nm compared with BiOCl prepared without the assistance of black phosphorus, and the excessive preparation of black phosphorus can inhibit the surface photovoltage signal of BiOCl.
Example 7
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 60mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 1.9%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 12 hours at 190 ℃, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In comparison with comparative example 1, black phosphorus was added at a black phosphorus/BiOCl mass ratio of 1.9% and a hydrothermal temperature of 190 ℃ and a hydrothermal time of 12 hours.
FIG. 7 is a graph showing comparison of surface photovoltage signals of samples obtained in example 7 and comparative example 1. As can be seen from FIG. 7, the BiOCl prepared with the assistance of black phosphorus has a weaker surface photovoltage signal in the range of 300-400nm than that of BiOCl prepared without the assistance of black phosphorus, and the preparation of black phosphorus with excessive hydrothermal temperature is used for inhibiting the surface photovoltage signal of BiOCl.
Example 8
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing orthorhombic black phosphorus in 50mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of black phosphorus to generated BiOCl is 0.5%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 24 hours at 135 ℃, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In contrast to comparative example 1, black phosphorus was added at a black phosphorus/BiOCl mass ratio of 0.5% with a hydrothermal temperature of 135 ℃ and a hydrothermal time of 24 hours.
FIG. 8 is a graph showing comparison of surface photovoltage signals of samples obtained in example 8 and comparative example 1. As can be seen from FIG. 8, the BiOCl prepared with the assistance of black phosphorus has weaker surface photovoltage signal in the range of 300-400nm than that of BiOCl prepared without the assistance of black phosphorus, and the BiOCl prepared with the assistance of black phosphorus has weaker surface photovoltage signal at too low hydrothermal temperature.
Example 9
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing red phosphorus in 50mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g of bismuth nitrate in a red phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the red phosphorus to the generated BiOCl is 1%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-red phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
Compared with comparative example 1, red phosphorus was added with a mass ratio of 1% red phosphorus/BiOCl.
FIG. 9 is a graph showing comparison of surface photovoltage signals of samples obtained in example 9 and comparative example 1. As can be seen from FIG. 9, the BiOCl prepared with the aid of red phosphorus has weaker surface photovoltage signal in the range of 300-400nm than that of BiOCl prepared without the aid of red phosphorus, and the BiOCl prepared with the aid of red phosphorus has weaker surface photovoltage signal.
Example 10
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing red phosphorus in 50mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g of bismuth nitrate in a red phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the red phosphorus to the generated BiOCl is 1.5%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-red phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 24 hours, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In contrast to comparative example 1, red phosphorus was added at a red phosphorus/BiOCl mass ratio of 1.5% and a hydrothermal reaction temperature of 160 ℃.
FIG. 10 is a graph showing comparison of surface photovoltage signals of samples obtained in example 10 and comparative example 1. As can be seen from FIG. 10, the BiOCl prepared with the assistance of red phosphorus has weaker surface photovoltage signal in the range of 300-400nm than that of BiOCl prepared without the assistance of red phosphorus, and the BiOCl prepared with the assistance of red phosphorus has weaker surface photovoltage signal.
Example 11
The specific preparation process of the surface photovoltage signal weakening BiOCl in the embodiment is as follows:
1) Dispersing red phosphorus in 50mL glacial acetic acid, carrying out ultrasonic treatment for 10 minutes, dissolving 5g of bismuth nitrate in a red phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the red phosphorus to the generated BiOCl is 0.5%; and (3) dropwise adding 10mL of KCl solution into the bismuth nitrate-glacial acetic acid-red phosphorus suspension, wherein the mole number of KCl is equal to that of bismuth nitrate, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 24 hours at 150 ℃, and naturally cooling to room temperature.
2) Washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60deg.C to obtain sample.
In contrast to comparative example 1, red phosphorus was added at a red phosphorus/BiOCl mass ratio of 0.5% and a hydrothermal treatment temperature of 150 ℃.
FIG. 11 is a graph showing comparison of surface photovoltage signals of samples obtained in example 11 and comparative example 1. As can be seen from FIG. 11, the BiOCl prepared with the aid of red phosphorus has weaker surface photovoltage signal in the range of 300-400nm than that of BiOCl prepared without the aid of red phosphorus, and the BiOCl prepared with the aid of red phosphorus has weaker surface photovoltage signal.
The above description is illustrative of exemplary embodiments of the invention and is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (6)
1. A method for improving a BiOCl surface photovoltage signal, comprising the steps of:
the first step: dispersing black phosphorus in glacial acetic acid to prepare a black phosphorus-glacial acetic acid suspension system; dissolving bismuth nitrate in a black phosphorus-glacial acetic acid suspension system to obtain bismuth nitrate-glacial acetic acid-black phosphorus suspension; the black phosphorus is orthorhombic black phosphorus; the mass ratio of the black phosphorus to the BiOCl is 0.1% -1.9%;
and a second step of: dropwise adding KCl solution into bismuth nitrate-glacial acetic acid-black phosphorus suspension, transferring the generated precipitate into a hydrothermal reaction kettle for hydrothermal treatment, and naturally cooling to room temperature after finishing the hydrothermal treatment to obtain a sample; the hydrothermal treatment condition is that the temperature is 140-180 ℃ and the treatment time is 12-24 hours;
and a third step of: and washing the sample with deionized water, washing with alcohol, and vacuum drying to obtain BiOCl with improved surface photovoltage signal.
2. A method of increasing a BiOCl surface photovoltage signal according to claim 1, wherein: the ratio of the adding amount g of bismuth nitrate to the volume mL of glacial acetic acid is 1:8-12.
3. A method of increasing a BiOCl surface photovoltage signal according to claim 1, wherein: the mole number of KCl is equal to the mole number of bismuth nitrate.
4. A method of increasing a BiOCl surface photovoltage signal according to claim 1, wherein: the temperature of the vacuum drying was 60.+ -. 5 ℃.
5. A method of increasing a BiOCl surface photovoltage signal according to any one of claims 1-4, wherein: the number of times of alcohol washing is 1-2 times.
6. The BiOCl prepared by the method for improving the surface photovoltage signal of the BiOCl according to claim 1, which is characterized in that: the surface photovoltage signal of the BiOCl is obviously enhanced in the range of 300-400 nm.
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