CN113457698A - Method for improving BiOCl surface photovoltage signal - Google Patents
Method for improving BiOCl surface photovoltage signal Download PDFInfo
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- CN113457698A CN113457698A CN202110667730.7A CN202110667730A CN113457698A CN 113457698 A CN113457698 A CN 113457698A CN 202110667730 A CN202110667730 A CN 202110667730A CN 113457698 A CN113457698 A CN 113457698A
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 111
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 40
- 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 34
- 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 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001291 vacuum drying Methods 0.000 claims abstract description 17
- 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
- 238000002360 preparation method Methods 0.000 claims description 23
- 229910052797 bismuth Inorganic materials 0.000 claims description 17
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 17
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 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
- 239000012467 final product Substances 0.000 description 12
- 238000009210 therapy by ultrasound Methods 0.000 description 11
- 230000002238 attenuated effect Effects 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000000926 separation method Methods 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
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting 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
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 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
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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
- 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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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; adding bismuth nitrate, dissolving in the suspension of black phosphorus and glacial acetic acid, and adding a KCl solution dropwise (the molar number of KCl is equal to that of bismuth nitrate). And 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 performing vacuum drying to obtain the sample. The surface photovoltage signal of the BiOCl sample prepared by the assistance of a proper amount of black phosphorus is obviously enhanced in the range of 300-400 nm. The invention has simple and convenient 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 ternary oxide composed of V-VI-VII main group elements, the crystal structure belongs to a PbFCl type layered structure, the high anisotropy and the wide forbidden band width are 3.0-3.5 eV, and the BiOCl has a special layered structure and a proper forbidden band width, so that the BiOCl becomes an excellent oxideOne of the photocatalytic materials. Electrons on the valence band of the BiOCl photocatalyst under excitation of light of sufficient energy (e)-) Sufficient energy is absorbed to transition through the forbidden band to the conduction band, leaving a photovoid (h) in the valence band+) Thus, photo-generated electron-hole pairs (e) are formed--h+). The electrons transferred to the surface of the BiOCl undergo a reduction reaction with the organic matter adsorbed on the surface, and the holes undergo an oxidation reaction with the organic matter adsorbed on the surface.
The recombination reaction between the photo-generated electrons and the holes can release energy in the form of light or heat, and the photocatalytic performance of the photocatalyst is greatly reduced. Therefore, the photocatalytic efficiency of BiOCl is mainly affected by the frequency and intensity of incident light, the forbidden bandwidth of the photocatalyst, and the recombination rate of photo-generated electrons and holes.
The photocatalytic reaction occurs on the surface of the photocatalyst, and the surface property of the photocatalyst can obviously influence the separation efficiency of photo-generated charges, thereby influencing the photocatalytic activity. Therefore, the surface modification is an effective means for improving the photocatalytic activity of BiOCl. However, no better method for surface modification has been available.
Disclosure of Invention
The invention aims to solve the problems and provides a method for improving a BiOCl surface photovoltage signal, which can enhance the BiOCl surface photovoltage signal through black phosphorus assisted and appropriate black phosphorus surface modification; the black phosphorus surface modification can affect the growth of BiOCl and construct defects, the defects can capture photo-generated electrons and inhibit the recombination of the photo-generated electrons and holes, and the BiOCl with the enhanced surface photovoltage signals is obtained.
In order to achieve the above purpose, the specific technical scheme of the invention is as follows:
a method of increasing a BiOCl surface photovoltage signal, comprising the steps of:
1) dispersing a proper amount of black phosphorus in glacial acetic acid to obtain a black phosphorus-glacial acetic acid suspension system; and dissolving bismuth nitrate in a black phosphorus-glacial acetic acid suspension system to obtain bismuth nitrate-glacial acetic acid-black phosphorus suspension.
2) Dropwise adding a KCl solution into the 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 of the present application, the black phosphorus is orthorhombic black phosphorus.
In a preferred embodiment of the present invention, the ratio of the amount of bismuth nitrate added g to the volume of glacial acetic acid mL is 1: 8-12.
In a preferred embodiment of the present invention, the mass ratio of black phosphorus to generated BiOCl is 0.1% to 1.9%.
As a preferred embodiment of the present invention, the hydrothermal reaction is carried out at a temperature of 140 ℃ to 180 ℃ for 12 to 24 hours.
In a preferred embodiment of the present invention, the number of alcohol washes is 1 to 2.
As a preferred embodiment of the present application, the temperature of the vacuum drying is 60. + -. 5 ℃.
The BiOCl prepared by the method has the advantage that the surface photovoltage signal is obviously enhanced in the range of 300-400 nm.
The principle of this application does: black phosphorus is a solid having a metallic luster, has a wavy layered structure, has weaker bonding between layers than bonding within layers, and has conductivity. The application uses a proper amount of black phosphorus surface modified BiOCl to construct defects, and simultaneously improves the separation of photo-generated charges by utilizing the conductivity of the black phosphorus, and shows a higher surface photovoltage signal.
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 surface photovoltage signal of BiOCl obtained by surface modification of a proper amount of black phosphorus in the range of 300-400nm is obviously enhanced, 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 addition and the samples obtained in example 1.
FIG. 2 is a comparison of the surface photovoltage signals of BiOCl prepared without adding black phosphorus and the samples obtained in example 2.
FIG. 3 is a comparison of the surface photovoltage signals of BiOCl prepared without adding black phosphorus and the samples obtained in example 3.
FIG. 4 is a comparison of the surface photovoltage signals of BiOCl prepared without adding 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 addition and the samples obtained in example 5.
FIG. 6 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus addition and the samples obtained in example 6.
FIG. 7 is a comparison of the surface photovoltage signals of BiOCl prepared without adding black phosphorus and the samples obtained in example 7.
FIG. 8 is a comparison of the surface photovoltage signals of BiOCl prepared without black phosphorus addition and the samples obtained in example 8.
FIG. 9 is a comparison of the surface photovoltage signals of BiOCl prepared without addition of red phosphorus and the samples obtained in example 9.
FIG. 10 is a comparison of the surface photovoltage signals of BiOCl prepared without addition of red phosphorus and the samples obtained in example 10.
FIG. 11 is a comparison of the surface photovoltage signals of BiOCl prepared without addition of red phosphorus and the samples obtained in example 11.
Detailed Description
A method of increasing a BiOCl surface photovoltage signal, comprising the steps of:
the first step is as follows: dispersing a proper amount of black phosphorus in glacial acetic acid, and dissolving bismuth nitrate in a black phosphorus-glacial acetic acid suspension system; preferably, the volume ratio of bismuth nitrate/glacial acetic acid: 5g/40mL-5g/60mL, and the mass ratio of the black phosphorus to the BiOCl is 0.1-1.9%.
The second step is that: dropwise adding a KCl solution into the bismuth nitrate-glacial acetic acid-black phosphorus suspension, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 140 ℃ and 180 ℃ for 12-24 hours, and naturally cooling to room temperature.
The third step: washing the sample with deionized water, washing with alcohol for 1-2 times, and vacuum drying at 60 deg.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 the surface photovoltage signal obviously enhanced in the range of 300-400nm
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the following examples, the surface photovoltage test is performed on a surface photovoltage spectrum assembled in Jilin university, a xenon lamp is used as a light source, a lock-in amplifier is used for amplifying the acquired signal, a sample is pressed between conductive glass and a metal copper base, the wavelength test range is 300-400nm, and the specific test method and the operation adopt conventional technical means.
Comparative example 1
1) Dissolving 5g of bismuth nitrate in 40mL of glacial acetic acid; to the bismuth nitrate-glacial acetic acid solution was added dropwise 10mL of KCl solution, 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 at 180 ℃ for 24 hours, and naturally cooling to room temperature.
2) And (3) carrying out suction filtration and deionized water washing, then washing for 1-2 times by using alcohol, carrying out vacuum drying on the obtained solid at 60 ℃, taking out and grinding the obtained solid, and testing an optical voltage signal.
Example 1
The preparation process of the surface photovoltage signal enhanced BiOCl in the embodiment is as follows:
1) dispersing orthorhombic black phosphorus in 40mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 0.1%; 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 60 deg.C to obtain the final product.
In comparison with comparative example 1, black phosphorus was added in a mass ratio of black phosphorus/BiOCl of 0.1%.
FIG. 1 is a graph comparing the surface photovoltage signals of the samples obtained in example 1 and comparative example 1. As can be seen from FIG. 1, BiOCl prepared by black phosphorus assistance is significantly enhanced in the range of 300-400nm compared with BiOCl surface photovoltage signals which are not prepared by black phosphorus assistance, and proper black phosphorus assistance preparation can enhance BiOCl surface photovoltage signals.
Example 2
The specific preparation process of the surface photovoltage signal enhanced BiOCl in this embodiment is as follows:
1) dispersing orthorhombic black phosphorus in 50mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 0.5%; 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the generated BiOCl is 0.5 percent, the hydrothermal temperature is 140 ℃, and the hydrothermal time is 12 hours.
Fig. 2 is a graph comparing surface photovoltage signals of samples obtained in example 2 and comparative example 1. As can be seen from FIG. 2, BiOCl prepared by black phosphorus assistance is significantly enhanced in the range of 300-400nm compared with BiOCl surface photovoltage signals which are not prepared by black phosphorus assistance, and proper black phosphorus assistance preparation can enhance BiOCl surface photovoltage signals.
Example 3
The specific preparation process of the surface photovoltage signal enhanced BiOCl in this embodiment is as follows:
1) dispersing orthorhombic black phosphorus in 60mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 1%; 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the generated BiOCl is 1%, the hydrothermal temperature is 160 ℃, and the hydrothermal time is 18 h.
Fig. 3 is a graph comparing surface photovoltage signals of samples obtained in example 3 and comparative example 1. As can be seen from FIG. 3, BiOCl prepared by black phosphorus assistance is significantly enhanced in the range of 300-400nm compared with BiOCl surface photovoltage signals which are not prepared by black phosphorus assistance, and proper black phosphorus assistance preparation can enhance BiOCl surface photovoltage signals.
Example 4
The specific preparation process of the surface photovoltage signal enhanced BiOCl in this embodiment is as follows:
1) dispersing orthorhombic black phosphorus in 45mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 1.5%; 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the generated BiOCl is 1.5%, the hydrothermal temperature is 180 ℃, and the hydrothermal time is 12 h.
Fig. 4 is a graph comparing surface photovoltage signals of samples obtained in example 4 and comparative example 1. As can be seen from FIG. 4, BiOCl prepared by black phosphorus assistance is significantly enhanced in the range of 300-400nm compared with BiOCl surface photovoltage signals which are not prepared by black phosphorus assistance, and proper black phosphorus assistance preparation can enhance BiOCl surface photovoltage signals.
Example 5
The specific preparation process of the surface photovoltage signal enhanced BiOCl in this embodiment is as follows:
1) dispersing orthorhombic black phosphorus in 45mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 1.9%; 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 20 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the generated BiOCl is 1.9%, the hydrothermal temperature is 140 ℃, and the hydrothermal time is 20 h.
Fig. 5 is a graph comparing surface photovoltage signals of samples obtained in example 5 and comparative example 1. As can be seen from FIG. 5, BiOCl prepared by black phosphorus assistance is significantly enhanced in the range of 300-400nm compared with BiOCl surface photovoltage signals which are not prepared by black phosphorus assistance, and proper black phosphorus assistance preparation can enhance BiOCl surface photovoltage signals.
Example 6
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing orthorhombic black phosphorus in 55mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 2%; 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the BiOCl is 2%, the hydrothermal temperature is 140 ℃, and the hydrothermal time is 20 hours.
Fig. 6 is a graph comparing surface photovoltage signals of samples obtained in example 6 and comparative example 1. As can be seen from FIG. 6, the BiOCl prepared by black phosphorus assistance is weaker than the BiOCl surface photovoltage signal which is not prepared by black phosphorus assistance in the range of 300-400nm, and the excessive black phosphorus assistance preparation can inhibit the BiOCl surface photovoltage signal.
Example 7
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing orthorhombic black phosphorus in 60mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 1.9%; 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 190 ℃ 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the BiOCl is 1.9%, the hydrothermal temperature is 190 ℃, and the hydrothermal time is 12 hours.
Fig. 7 is a graph comparing surface photovoltage signals of samples obtained in example 7 and comparative example 1. As can be seen from FIG. 7, the BiOCl prepared by black phosphorus assistance is weaker than the BiOCl surface photovoltage signal which is not prepared by black phosphorus assistance in the range of 300-400nm, and the black phosphorus assistance preparation for inhibiting the BiOCl surface photovoltage signal when the hydrothermal temperature is too high.
Example 8
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing orthorhombic black phosphorus in 50mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and dissolving 5g of bismuth nitrate in a black phosphorus-glacial acetic acid suspension system, wherein the mass ratio of the black phosphorus to the generated BiOCl is 0.5%; 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 135 ℃ 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, the black phosphorus is added, the mass ratio of the black phosphorus to the BiOCl is 0.5%, the hydrothermal temperature is 135 ℃, and the hydrothermal time is 24 hours.
Fig. 8 is a graph comparing surface photovoltage signals of samples obtained in example 8 and comparative example 1. As can be seen from fig. 8, the BiOCl prepared by black phosphorus assistance is weaker than the BiOCl surface photovoltage signal prepared without black phosphorus assistance in the range of 300-400nm, and the BiOCl surface photovoltage signal prepared by black phosphorus assistance at too low hydrothermal temperature is weaker.
Example 9
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing red phosphorus in 50mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and 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%; 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 60 deg.C to obtain the final product.
In comparison with comparative example 1, red phosphorus was added in a mass ratio of red phosphorus/BiOCl of 1%.
Fig. 9 is a graph comparing 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 assistance of red phosphorus is weaker than the BiOCl surface photovoltage signal not prepared with the assistance of red phosphorus in the range of 300-400nm, and the BiOCl surface photovoltage signal prepared with the assistance of red phosphorus is weaker.
Example 10
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing red phosphorus in 50mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and 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%; 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, red phosphorus is added, the mass ratio of red phosphorus to BiOCl is 1.5%, and the hydrothermal reaction temperature is 160 ℃.
Fig. 10 is a graph comparing 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 is weaker than the BiOCl surface photovoltage signal not prepared with the assistance of red phosphorus in the range of 300-400nm, and the BiOCl surface photovoltage signal prepared with the assistance of red phosphorus is weaker.
Example 11
The specific preparation process of the surface photovoltage signal-attenuated BiOCl of this example is as follows:
1) dispersing red phosphorus in 50mL of glacial acetic acid, performing ultrasonic treatment for 10 minutes, and 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%; 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 150 ℃ 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 60 deg.C to obtain the final product.
Compared with the comparative example 1, red phosphorus is added, the mass ratio of red phosphorus to BiOCl is 0.5%, and the hydrothermal treatment temperature is 150 ℃.
FIG. 11 is a graph comparing the surface photovoltage signals of the samples obtained in example 11 and comparative example 1. As can be seen from fig. 11, the BiOCl prepared with the assistance of red phosphorus is weaker than the BiOCl surface photovoltage signal not prepared with the assistance of red phosphorus in the range of 300-400nm, and the BiOCl surface photovoltage signal prepared with the assistance of red phosphorus is weaker.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for improving a BiOCl surface photovoltage signal is characterized by comprising the following steps:
the first step is as follows: 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 second step is that: dropwise adding a KCl solution into the 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 the hydrothermal treatment to obtain a sample;
the third step: and washing the sample with deionized water, then washing with alcohol, and drying in vacuum to obtain the BiOCl with the improved surface photovoltage signal.
2. The preparation method for improving the BiOCl surface photovoltage signal as claimed in claim 1, wherein: the black phosphorus is orthorhombic black phosphorus; the mass ratio of the black phosphorus to the BiOCl is 0.1-1.9%.
3. The preparation method for improving the BiOCl surface photovoltage signal as claimed in claim 1, wherein: the proportion relationship of the addition amount g of the bismuth nitrate and the volume mL of the glacial acetic acid is 1: 8-12.
4. A method of producing an enhanced BiOCl surface photovoltage signal in accordance with claim 1, wherein: the moles of KCl are equal to the moles of bismuth nitrate.
5. The preparation method for improving the BiOCl surface photovoltage signal as claimed in claim 1, wherein: the hydrothermal treatment is carried out at 140 ℃ and 180 ℃ for 12-24 hours.
6. The preparation method for improving the BiOCl surface photovoltage signal as claimed in claim 1, wherein: the temperature for vacuum drying is 60 +/-5 ℃.
7. The method for preparing a BiOCl surface photovoltage signal according to any one of claims 1-6, wherein: the number of alcohol washes is 1-2.
8. The preparation method for improving the BiOCl surface photovoltage signal as claimed in claim 1, wherein: the BiOCl prepared by the method has obviously enhanced surface photovoltage signals in the range of 300-400 nm.
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