CN114225951B - Processing method of surface photovoltage signal enhanced BiOCl - Google Patents
Processing method of surface photovoltage signal enhanced BiOCl Download PDFInfo
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- CN114225951B CN114225951B CN202111497952.5A CN202111497952A CN114225951B CN 114225951 B CN114225951 B CN 114225951B CN 202111497952 A CN202111497952 A CN 202111497952A CN 114225951 B CN114225951 B CN 114225951B
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 238000003672 processing method Methods 0.000 title claims abstract description 12
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 66
- 238000001035 drying Methods 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 238000000967 suction filtration Methods 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 18
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 22
- 230000009286 beneficial effect Effects 0.000 description 9
- 239000011941 photocatalyst Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 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
- 239000002178 crystalline material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- -1 superoxide anions Chemical class 0.000 description 1
- 238000010998 test method Methods 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The application belongs to the technical field of photocatalytic materials, and particularly relates to a processing method of surface photovoltage signal enhancement type BiOCl used in the field of photocatalysis. Dispersing a proper amount of BiOCl in deionized water, and carrying out hydrothermal treatment after stirring; 2) Filtering, washing, transferring and drying, and grinding the solid to obtain the photo-voltage signal enhanced BiOCl. The processing method of the BiOCl with the obviously enhanced surface photovoltage signal is simple and convenient to operate, does not add any other chemical, is easy to realize, and is safe and reliable. Compared with the BiOCl without hydrothermal treatment, with overhigh hydrothermal treatment temperature or overlong hydrothermal treatment time, the surface photovoltage signal of the BiOCl in the interval of 300-400 nm is obviously enhanced, and the method has important practical significance for improving the photo-generated electron-hole separation.
Description
Technical Field
The application belongs to the technical field of photocatalytic materials, and particularly relates to a processing method of surface photovoltage signal enhancement type BiOCl used in the field of photocatalysis.
Background
Semiconductor photocatalysis is a promising technology for storing photon energy in chemical bonds using solar energy to mitigate environmental degradation and alleviate energy crisis. Among the photocatalysts developed at present, biOCl has been attracting research interest of researchers due to its characteristics of high activity, practicality, stability, low cost, etc. BiOCl has a special [ Cl-Bi-O-Bi-Cl ] layered structure, which aids in the separation of photogenerated electrons and holes. The BiOCl band gap is 3.4eV, belongs to a wide-band semiconductor, and can only absorb ultraviolet light accounting for less than 5% of the total solar spectrum, so that the utilization rate of sunlight is low, and how to improve the photocatalytic activity of BiOCl gradually becomes a research hot spot. In addition, the rapid recombination of the BiOCl photogenerated electrons and holes makes it far from satisfactory for practical use.
The photocatalytic reaction is a series of comprehensive processes, including photoelectric conversion process, material structure change, redox chemical reaction, etc. For a BiOCl photocatalyst, photons of appropriate energy are incident on its surface, exciting photoelectrons of a certain energy, and leaving holes in situ in the BiOCl crystalline material. Electrons excited in the valence band (e - ) Will initiate a reduction reaction, while holes (h) + ) The oxidation reaction is initiated. The photogenerated electrons and holes are collectively called carriers, and the photogenerated electrons react with oxygen to generate superoxide anions (e - +O 2 =·O 2 - ) The hole oxidizes water to form a hydroxyl radical (·oh) which in turn undergoes a series of photocatalytic reactions.
Among the many factors affecting photocatalytic activity, the separation speed of photogenerated electrons-holes plays a very important role. The stronger the surface photovoltage signal is, the faster the photo-generated electron-hole separation speed is, and the higher the corresponding photocatalytic performance is. Therefore, improving the separation speed of photo-induced electrons and holes of the BiOCl photocatalyst is an important means for improving the photocatalytic activity, and has great significance for realizing the industrial application of the BiOCl photocatalyst.
Disclosure of Invention
The application aims to provide a processing method of surface photovoltage signal enhancement type BiOCl. In the method, the BiOCl powder can obviously enhance the surface photovoltage signal after proper hydrothermal treatment; under the condition of illumination, the semiconductor photocatalyst can generate electron-hole pairs to form surface photovoltage. The magnitude of the surface photovoltage is closely related to the photocatalyst surface state.
In order to achieve the above object, the present application has the technical scheme that:
a processing method of surface photovoltage signal enhancement type BiOCl comprises the following steps:
1) And dispersing the BiOCl solid in deionized water, stirring, transferring to a hydrothermal reaction kettle, and carrying out hydrothermal treatment.
2) Filtering, washing, transferring and drying, and grinding the solid to obtain the photo-voltage signal enhanced BiOCl.
As a better implementation mode in the application, the ratio relation between the mass g of the BiOCl in the step 1) and the volume mL of deionized water is 3:60-3:30; more preferably 3:55.
In a preferred embodiment of the present application, the stirring time is about 0.5 hours.
As a preferred embodiment of the present application, the hydrothermal treatment temperature in step 1) is 120-180 ℃ and the time is 0.5-30 h. Still more preferably, the temperature of the hydrothermal treatment is 170℃and the time is 24 hours.
In a preferred embodiment of the present application, in the step 2), the drying temperature is 60 to 100 ℃ and the time is 12 to 14 hours. Even more preferably, the drying temperature is 75℃and the time is 12 hours.
The surface photovoltage signal enhanced BiOCl is obtained by adopting the processing method; the surface photovoltage signal enhancement BiOCl obtained by treatment obviously enhances the surface photovoltage signal in the interval of 300-400 nm.
Compared with the prior art, the application has the following beneficial effects:
the processing method of the BiOCl with the obviously enhanced surface photovoltage signal is simple and convenient to operate, does not need additional chemicals, is easy to realize, and is safe and reliable.
And secondly, compared with BiOCl which is not subjected to hydrothermal treatment, has overhigh hydrothermal temperature or overlong hydrothermal treatment time, the BiOCl subjected to moderate hydrothermal treatment has obviously enhanced surface photovoltage signals in a range of 300-400 nm, and has important practical significance for improving the photocatalytic activity.
Drawings
FIG. 1 is an XRD pattern of a BiOCl sample without hydrothermal treatment (comparative).
FIG. 2 is a graph comparing the surface photovoltage signals of the samples obtained in example 1 and BiOCl without hydrothermal treatment.
FIG. 3 is a graph comparing surface photovoltage signals of samples obtained in example 2 and BiOCl without hydrothermal treatment.
FIG. 4 is a graph comparing the surface photovoltage signals of the samples obtained in example 3 and BiOCl without hydrothermal treatment.
FIG. 5 is a graph comparing the surface photovoltage signals of the samples obtained in example 4 and BiOCl without hydrothermal treatment.
FIG. 6 is a graph comparing surface photovoltage signals of samples obtained in example 5 and BiOCl without hydrothermal treatment.
FIG. 7 is a graph comparing surface photovoltage signals of samples obtained in example 6 and BiOCl without hydrothermal treatment.
FIG. 8 is a graph comparing surface photovoltage signals of samples obtained in example 7 and BiOCl without hydrothermal treatment.
FIG. 9 is a graph comparing surface photovoltage signals of samples obtained in example 8 and BiOCl without hydrothermal treatment.
FIG. 10 is a graph comparing the surface photovoltage signals of the samples obtained in example 9 and BiOCl without hydrothermal treatment.
FIG. 11 is a graph of surface photovoltage signal comparison of the samples obtained in example 10 and BiOCl without hydrothermal treatment.
Detailed Description
A processing method of surface photovoltage signal enhancement type BiOCl comprises the following steps:
1) And dispersing the BiOCl solid in deionized water, stirring, transferring to a hydrothermal reaction kettle, and carrying out hydrothermal treatment.
2) Filtering, washing, transferring and drying, and grinding the solid to obtain the photo-voltage signal enhanced BiOCl.
Preferably, the stirring time is 0.5h.
Preferably, the volume ratio of the mass of BiOCl to deionized water in the step 1) is 3g:60 mL-3 g:30m.
As a further preference, the volume ratio of BiOCl to deionized water is 3:55.
Preferably, the temperature of the hydrothermal treatment in the step 1) is 120-180 ℃ and the time is 0.5-30 h. Still more preferably, the temperature of the hydrothermal treatment is 170℃and the time is 24 hours.
Preferably, in the step 2), the drying temperature is 60-100 ℃ and the time is 12-14 h.
Even more preferably, the drying temperature is 75℃and the time is 12 hours.
The surface photovoltage signal enhanced BiOCl is obtained by adopting the processing method; the surface photovoltage signal is obviously enhanced in the interval of 300-400 nm.
The present application 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 application 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 application.
In the following examples, the BiOCl crystal phase is characterized by DX-2600X-ray powder diffraction; 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 300-400 nm, and the specific test method and operation adopt conventional technical means.
Comparative example 1
1) 3g of BiOCl was dispersed in 60mL deionized water and stirred for 0.5h.
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 60 ℃ for 12 hours, taking out the obtained solid, grinding, and testing the photovoltage signal.
FIG. 1 is an XRD pattern for BiOCl.
Example 1
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 30mL of deionized water, stirred for 0.5h and then transferred to a 100mL hydrothermal reaction kettle, and the mixture is heated to 120 ℃ in a hydrothermal manner and subjected to hydrothermal treatment for 0.5h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 60 ℃ for 12 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 1 had a hydrothermal temperature of 120℃and a hydrothermal treatment time of 0.5h.
FIG. 2 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. 2, biOCl is subjected to hydrothermal treatment at 120 ℃ for 0.5h, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm, and proper hydrothermal treatment can enhance the surface photovoltage signal, which is beneficial to improving the photocatalytic activity.
Example 2
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 40mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 140 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 4h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 70 ℃ for 14 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 2 had a hydrothermal temperature of 140℃and a hydrothermal treatment time of 4 hours. The drying temperature is 70 ℃ and the time is 14 hours.
FIG. 3 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. 3, the surface photovoltage signal of the BiOCl is obviously enhanced in the range of 340-400 nm after the BiOCl is subjected to the hydrothermal treatment for 4 hours at 140 ℃, and the surface photovoltage signal can be enhanced by proper hydrothermal treatment, which is beneficial to improving the photocatalytic activity.
Example 3
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 50mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 160 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 8h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 80 ℃ for 13 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 3 had a hydrothermal temperature of 160℃and a hydrothermal treatment time of 8 hours. The drying temperature is 80 ℃ and the drying time is 13h.
FIG. 4 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. 4, biOCl is subjected to the water heat treatment at 160 ℃ for 8 hours, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm, and the proper water heat treatment can enhance the surface photovoltage signal, which is beneficial to improving the photocatalytic activity.
Example 4
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 50mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 180 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 12h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 80 ℃ for 13 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 3 had a hydrothermal temperature of 180℃and a hydrothermal treatment time of 12 hours. The drying temperature is 80 ℃ and the drying time is 13h.
FIG. 5 is a graph showing comparison of surface photovoltage signals of the samples obtained in comparative example 1 and example 4. As can be seen from FIG. 5, biOCl is subjected to hydrothermal treatment at 180 ℃ for 12 hours, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm, and proper hydrothermal treatment can enhance the surface photovoltage signal, which is beneficial to improving the photocatalytic activity.
Example 5
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 30mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 120 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 16h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 65 ℃ for 14 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 5 had a hydrothermal temperature of 120℃and a hydrothermal treatment time of 16h. The drying temperature is 65 ℃ and the drying time is 14 hours.
FIG. 6 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. 6, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm after the BiOCl is subjected to the hydrothermal treatment for 16 hours at 120 ℃, and the surface photovoltage signal can be enhanced by proper hydrothermal treatment, which is beneficial to improving the photocatalytic activity.
Example 6
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 45mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 130 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 20h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 70 ℃ for 14 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 6 had a hydrothermal temperature of 130℃and a hydrothermal treatment time of 20h. The drying temperature is 70 ℃ and the time is 14 hours.
FIG. 7 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. 7, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm after the BiOCl is subjected to the hydrothermal treatment for 20 hours at 130 ℃, and the surface photovoltage signal can be enhanced by proper hydrothermal treatment, which is beneficial to improving the photocatalytic activity.
Example 7
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 55mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 170 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 24h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 75 ℃ for 12 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 7 had a hydrothermal temperature of 170℃and a hydrothermal treatment time of 24 hours. The drying temperature is 75 ℃ and the drying time is 12 hours.
FIG. 8 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. 8, biOCl is subjected to water heating treatment at 170 ℃ for 24 hours, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm, and proper water heating treatment can enhance the surface photovoltage signal, which is beneficial to improving the photocatalytic activity.
Example 8
The specific processing procedure of the surface photovoltage signal enhancement type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 60mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 180 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 30h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 80 ℃ for 12 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 8 had a hydrothermal temperature of 180℃and a hydrothermal treatment time of 30 hours. The drying temperature is 80 ℃ and the drying time is 12 hours.
FIG. 9 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. 9, the surface photovoltage signal of BiOCl is obviously enhanced in the range of 340-400 nm after the BiOCl is subjected to the hydrothermal treatment for 30 hours at 180 ℃, and the surface photovoltage signal can be enhanced by proper hydrothermal treatment, which is beneficial to improving the photocatalytic activity.
Example 9
The specific processing procedure of the surface photovoltage signal weakening type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 60mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 190 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 0.5h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 60 ℃ for 14 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal reduced BiOCl.
In contrast to comparative example 1, example 9 had a hydrothermal temperature of 190℃and a hydrothermal treatment time of 0.5h. The drying temperature is 60 ℃ and the drying time is 14 hours.
FIG. 10 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. 10, biOCl is subjected to the hydrothermal treatment at 190 ℃ for 0.5h, and the BiOCl surface photovoltage signal is obviously weakened in the range of 340-400 nm, which indicates that the surface photovoltage signal is reduced by the hydrothermal treatment at too high temperature.
Example 10
The specific processing procedure of the surface photovoltage signal weakening type BiOCl in this embodiment is as follows:
1) 3g of BiOCl is dispersed in 45mL of deionized water, stirred for 0.5h, transferred to a 100mL hydrothermal reaction kettle, heated to 120 ℃ in a hydrothermal manner, and subjected to hydrothermal treatment for 48h;
2) And (3) carrying out suction filtration, washing, transferring the obtained solid into an oven, drying at 80 ℃ for 13 hours, taking out the obtained solid, and grinding to obtain the photovoltage signal enhanced BiOCl.
In contrast to comparative example 1, example 10 had a hydrothermal temperature of 120℃and a hydrothermal treatment time of 48 hours. The drying temperature is 80 ℃ and the drying time is 13h.
FIG. 11 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. 11, the surface photovoltage signal of BiOCl is significantly reduced in the interval of 340-400 nm after the BiOCl is subjected to the hydrothermal treatment at 120 ℃ for 48 hours, which indicates that the surface photovoltage signal is significantly reduced after the hydrothermal treatment time is too long.
The above description is illustrative of exemplary embodiments of the application and is not intended to limit the application 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 application.
Claims (7)
1. The processing method of the surface photovoltage signal enhanced BiOCl is characterized by comprising the following steps of:
1) Dispersing BiOCl solid in deionized water, stirring, and transferring to a hydrothermal reaction kettle for hydrothermal treatment, wherein the hydrothermal treatment temperature is 120-180 ℃ and the time is 12-30 h;
2) Carrying out suction filtration, washing, transferring and drying on the substances subjected to the hydrothermal treatment, and grinding the solid to obtain the photo-voltage signal enhanced BiOCl; the surface photovoltage signal enhancement type BiOCl remarkably enhances the surface photovoltage signal in the interval of 300-400 nm.
2. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the ratio relation of the mass g of the BiOCl to the volume mL of the deionized water is 3:60-3:30.
3. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: the stirring time in step 1) was 0.5h.
4. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: in the step 2), the drying temperature is 60-80 ℃ and the time is 12-14 h.
5. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: in step 1), the ratio of the mass g of BiOCl to the volume mL of deionized water is 3:55.
6. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: the temperature of the hydrothermal treatment in the step 1) is 170 ℃, and the time of the hydrothermal treatment is 24 hours.
7. The method for processing the surface photovoltage signal enhancement type BiOCl as claimed in claim 1, wherein the method comprises the following steps: in the step 2), the drying temperature is 75 ℃ and the time is 12 hours.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202111497952.5A CN114225951B (en) | 2021-12-09 | 2021-12-09 | Processing method of surface photovoltage signal enhanced BiOCl |
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