CN107262120B - Preparation method for remarkably enhancing BiOCl surface photovoltage signals - Google Patents
Preparation method for remarkably enhancing BiOCl surface photovoltage signals Download PDFInfo
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- CN107262120B CN107262120B CN201710562338.XA CN201710562338A CN107262120B CN 107262120 B CN107262120 B CN 107262120B CN 201710562338 A CN201710562338 A CN 201710562338A CN 107262120 B CN107262120 B CN 107262120B
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- bismuth nitrate
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 54
- 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 description 53
- 229960000583 acetic acid Drugs 0.000 claims description 37
- 239000012362 glacial acetic acid Substances 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 29
- 229920001503 Glucan Polymers 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 229910052797 bismuth Inorganic materials 0.000 claims description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010335 hydrothermal treatment Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 32
- 229920002307 Dextran Polymers 0.000 description 29
- 239000000047 product Substances 0.000 description 19
- 238000012360 testing method Methods 0.000 description 10
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 208000017983 photosensitivity disease Diseases 0.000 description 1
- 231100000434 photosensitization Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-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
-
- B01J35/39—
-
- 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
Abstract
The invention relates to the field of material chemistry, in particular to the field of photocatalytic materials, and specifically relates to a preparation method for remarkably enhancing BiOCl surface photovoltage signals.
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 preparation method for remarkably enhancing BiOCl surface photovoltage signals.
Background
The crystal structure of BiOCl is PbFCl type, and the symmetry is D4hBiOCl has a layered structure, with the atoms of BiOCl in a bilayer arrangement being bound by Cl atoms through non-bonding forces (van der Waals forces). BiOCl valence bands are predominantly occupied by O2P and Cl 3P, and conduction bands are predominantly contributed by the Bi 6P orbital2BiOCl has a bandwidth of 3.22eV and exhibits a visible light catalytic activity of under visible light irradiation (λ > 420nm), which is mainly attributed to photosensitization degradation, and for practical applications, the photo-generated charge separation effect and the photo-catalytic activity of BiOCl are expected to be further improved is a very effective method for photocatalytic activity.
Research on the photocatalytic activity of the BiOCl-based heterojunction is carried out. Mushtaq and collaborator prepared Bi in situ2O3the/BiOCl heterojunction, they speculated on photo-generated charge transfer under visible light irradiation: under the irradiation of visible light Bi2O3Excited, electrons transit to conduction band to generate holes in valence band, and electrons on BiOCl valence band move to Bi under the action of interface electric field2O3The valence band shifts, thereby accumulating holes in the BiOCl valence band and Bi2O3The conduction band accumulates electrons, and the separation of photo-generated charges is effectively realized. The separated photo-generated charges induce a light-emitting catalytic reaction, so that the photocatalytic activity of the photo-generated charges is improved. The Guerrero subject group adopts a sol-gel method to load BiOCl on porous TiO2And the experimental result shows that the catalyst has enhanced photocatalytic activity on rhodamine B. Under UV-visible irradiation, TiO is different in band position2Electrons on the conduction band are transferred to the BiOCl conduction band, and holes on the BiOCl valence band are transferred to TiO2Valence band transfer, effective realization of photo-generated charge separation, and remarkable improvement of photo-catalytic activity thereof, the professor of Wangzhou daoyuan at Fuzhou university and the like adopt an pot hydrothermal method to prepare Bi3O4The result shows that Bi is contained in the Cl/BiOCl heterojunction3O4Cl/BiOCl heterojunction pure Bi3O4Cl and BiOCl have high photocatalytic activity, and when excited by visible light, Bi3O4The Cl is excited to generate holes and electrons. Electrons on the BiOCl valence band can be transferred to Bi under the action of an interface electric field3O4Cl valence band, thereby achieving effective separation of charges. Bi prepared by utilizing hydrothermal method by professor of Zhuyong method of Qinghua university2MoO6BiOCl heterojunction exhibiting a specific ratio to BiOCl, Bi2MoO6More excellent visible light catalytic activity. Under the irradiation of visible light, Bi2MoO6Generating electron-hole pairs due to Bi2MoO6Is more negative than the conduction band of BiOCl, Bi2MoO6The photo-generated electrons on the conduction band can be transferred to the conduction band of the BiOCl, so that the photo-generated electrons and holes are effectively separated, and the visible light of the photo-generated electrons and holes isThe catalytic activity is enhanced. The brave of Zhejiang university adopts ion exchange and 400 ℃ heating mode to prepare flower-shaped BiOCl/(BiO)2CO3/Bi2O3A heterojunction with photocatalytic activity higher than that of BiOCl/(BiO)2CO3And Bi2O3/(BiO)2CO3. Under the irradiation of visible light, methyl orange adsorbed on the surface of BiOCl is converted into an excited state, which injects electrons into the conduction band of BiOCl due to BiOCl and (BiO)2CO3Difference in conduction band position, BiOCl conduction band electronic orientation (BiO)2CO3And (4) transferring a conduction band. When Bi is present2O3Excited by visible light, conduction band electron direction (BiO)2CO3However, the above methods have the defects of complicated operation and poor controllability, and the simple and convenient means is urgently needed to improve the BiOCl photoproduction charge separation effect so as to further improve the photocatalysis performance and lay a solid foundation for realizing industrial application.
Disclosure of Invention
Based on the technical problems, the invention provides BiOCl surface photovoltage signal obviously-enhanced preparation methods, which are simple and convenient to operate, easy to obtain raw materials, easy to realize, safe and reliable, and compared with BiOCl prepared by a hydrothermal method without adding glucan 20000 for assisting, the BiOCl prepared by the hydrothermal method under the assistance of glucan 20000 obviously enhances the surface photovoltage signal in a range of 300-.
The specific technical scheme of the invention is as follows:
the preparation methods for remarkably enhancing BiOCl surface photovoltage signals are prepared by adopting the following steps:
, dissolving 5g of bismuth nitrate in 40-60mL of glacial acetic acid, and then adding glucan 20000 to obtain a bismuth nitrate-glacial acetic acid-glucan solution, wherein the molar ratio of glucan to bismuth nitrate is 1-11%.
The second step is that: and (3) dropwise adding a KCl solution into the bismuth nitrate-glacial acetic acid-glucan solution, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 160 ℃ and 180 ℃ for 24 hours, and naturally cooling to room temperature.
The third step: washing the sample with a large amount of deionized water, washing with alcohol for 1-2 times, taking out the powder, dispersing in alcohol, and drying at 60-80 deg.C to obtain the sample.
Preferably, the dextran is dextran 20000.
And washing the sample subjected to the hydrothermal reaction by using deionized water and ethanol, dispersing by using ethanol, and drying to obtain the sample. Wherein the mass concentration of the ethanol is about 95 percent.
The positive effects of the invention are as follows:
() compared with BiOCl prepared by hydrothermal method without glucan auxiliary, BiOCl prepared by hydrothermal method with glucan auxiliary is obviously enhanced in surface photovoltage signal in the range of 300-500nm, and even has obvious surface photovoltage signal in visible light region.
The invention adopts dextran 20000 for assistance, and prepares BiOCl with a significantly enhanced surface photovoltage signal by a hydrothermal method, and the prepared BiOCl shows higher photocatalytic activity.
Drawings
FIG. 1 is an XRD pattern of a product obtained in comparative example 1
FIG. 2 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 1
FIG. 3 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 2
FIG. 4 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 3
FIG. 5 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 4
FIG. 6 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 5
FIG. 7 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 6
FIG. 8 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 7
FIG. 9 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 8
FIG. 10 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 9
Detailed Description
The present invention is further illustrated by in the following examples and comparative examples, which are to be construed as merely illustrative and not limitative of the remainder of the disclosure, and it is to be understood that various changes and modifications can be effected therein by one skilled in the art after reading the teachings herein and that equivalents fall within the scope of the appended claims.
Comparative example 1:
at step , bismuth nitrate was dissolved in glacial acetic acid, specifically 5g of bismuth nitrate was dissolved in 40mL of glacial acetic acid.
And secondly, dropwise adding 10mLKCl solution into the bismuth nitrate-glacial acetic acid solution, wherein the molar number of KCl is equal to that of bismuth nitrate. Transferring the generated precipitate into a 100mL hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
FIG. 1 is an XRD spectrum of a sample obtained in comparative example 1, and it can be seen that the diffraction peak of the prepared sample was completely with that of a standard card (No.06-0249), indicating that the sample was BiOCl and had a higher purity.
Example 1:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 40mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 1% of that of the bismuth nitrate.
In the second step, 10mL of KCl solution, the number of moles of which is equal to that of bismuth nitrate, was added dropwise to the bismuth nitrate-glacial acetic acid solution. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 2 added dextran 20000, the dextran moles being 1% of the bismuth nitrate.
FIG. 2 is a graph comparing the surface photovoltage signals of the products obtained in comparative example 1 and example 1. It can be seen that after the dextran 20000 assists the hydrothermal reaction, the BiOCl surface photovoltage signal is significantly enhanced in the range of 300-400 nm. And in the range of 400-450nm, the surface photovoltage signal is enhanced, which shows that the visible light can excite the prepared photocatalyst to generate the surface photovoltage signal, which is beneficial to improving the visible light catalytic activity.
Example 2:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 50mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 3% of that of the bismuth nitrate.
In the second step, 10mL of KCl solution, the number of moles of which is equal to that of bismuth nitrate, was added dropwise to the bismuth nitrate-glacial acetic acid solution. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 160 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with alcohol for 1-2 times after washing with deionized water, taking out the powder, dispersing in alcohol, drying at 60 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 2 added dextran 20000, the dextran mole number being 3% of that of bismuth nitrate, the hydrothermal temperature being 160 ℃, the glacial acetic acid volume being 50mL, the drying temperature being 60 ℃.
FIG. 3 is a graph comparing the surface photovoltage signals of the products obtained in comparative example 1 and example 2. After the dextran 20000 assists the hydrothermal reaction, the BiOCl surface photovoltage signal is obviously enhanced in the range of 300-400 nm. And in the region of 425-475nm, the surface photovoltage signal is enhanced, which shows that the visible light can excite the prepared photocatalyst to generate the surface photovoltage signal, which is beneficial to improving the visible light catalytic activity.
Example 3:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 60mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 4% of that of the bismuth nitrate.
And secondly, dropwise adding 10mLKCl solution into the bismuth nitrate-glacial acetic acid solution, wherein the molar number of KCl is equal to that of bismuth nitrate. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 170 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with alcohol for 1-2 times after washing with deionized water, taking out the powder, dispersing in alcohol, drying at 70 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 3 added dextran 20000, the dextran mole number being 4% of that of bismuth nitrate, the hydrothermal temperature being 170 ℃, the glacial acetic acid volume being 60mL and the drying temperature being 70 ℃.
FIG. 4 is a graph comparing the surface photovoltage signals of the products obtained in comparative example 1 and example 2. After the dextran 20000 is added to assist the hydrothermal reaction, the BiOCl surface photovoltage signal is obviously enhanced in the range of 300-400 nm. And in the region of 425-475nm, the surface photovoltage signal is enhanced, which indicates that the visible light can excite the prepared photocatalyst to generate the surface photovoltage signal.
Example 4:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 45mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 7% of that of the bismuth nitrate.
And secondly, dropwise adding 10mLKCl solution into the bismuth nitrate-glacial acetic acid solution, wherein the molar number of KCl is equal to that of bismuth nitrate. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 165 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with alcohol for 1-2 times after washing with deionized water, taking out the powder, dispersing in alcohol, drying at 65 ℃ to obtain a sample, and testing the surface photovoltage.
In comparison with example 1, comparative example 2 added dextran 20000, the dextran mole number is 7% of bismuth nitrate, the hydrothermal temperature is 165 ℃, the glacial acetic acid volume is 45mL, and the drying temperature is 65 ℃.
Fig. 5 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 4. After the dextran 20000 is added to assist the hydrothermal reaction, the BiOCl surface photovoltage signal is obviously enhanced in the range of 300-375 nm.
Example 5
And , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 55mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 9% of that of the bismuth nitrate.
And secondly, dropwise adding 10mLKCl solution into the bismuth nitrate-glacial acetic acid solution, wherein the molar number of KCl is equal to that of bismuth nitrate. Transferring the generated precipitate into a 100mL hydrothermal reaction kettle, carrying out hydrothermal treatment at 175 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with alcohol for 1-2 times after washing with deionized water, taking out the powder, dispersing in alcohol, drying at 75 ℃ to obtain a sample, and testing the surface optical voltage.
In contrast to comparative example 1, example 5 added dextran 20000, the dextran mole number being 9% of that of bismuth nitrate, the hydrothermal temperature being 175 ℃, the glacial acetic acid volume being 55mL, the drying temperature being 75 ℃.
FIG. 6 is a graph comparing the surface photovoltage signals of the products obtained in comparative example 1 and example 5. After the dextran 20000 is added to assist the hydrothermal reaction, the BiOCl surface photovoltage signal is obviously enhanced in the range of 300-375 nm.
Example 6
And , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 60mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 11% of that of the bismuth nitrate.
And secondly, dropwise adding 10mLKCl solution into the bismuth nitrate-glacial acetic acid solution, wherein the molar number of KCl is equal to that of bismuth nitrate. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 6 added dextran 20000, the dextran moles being 11% of that of bismuth nitrate.
Fig. 7 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and comparative example 6. After the dextran 20000 is added to assist the hydrothermal reaction, the surface photovoltage signal of BiOCl in the range of 300-450nm is obviously enhanced, and the enhanced surface photovoltage is beneficial to improving the photocatalytic activity.
Example 7:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 60mL of glacial acetic acid, and adding 20000 parts of glucan, wherein the mole number of the glucan is 13% of that of the bismuth nitrate.
In the second step, 10mL of KCl solution, the number of moles of which is equal to that of bismuth nitrate, was added dropwise to the bismuth nitrate-glacial acetic acid solution. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 7 added dextran 20000, the dextran moles being 13% of the bismuth nitrate.
FIG. 8 is a graph comparing the surface photovoltage signals of the products obtained in comparative example 1 and example 7. It can be seen that after the dextran 20000 assists the hydrothermal reaction, the BiOCl surface photovoltage signals have no obvious difference in the 300-400nm interval in consideration of the measurement error.
Example 8:
and , dissolving bismuth nitrate in glacial acetic acid, specifically dissolving 5g of bismuth nitrate in 50mL of glacial acetic acid, and adding 20000 dextran, wherein the mole number of the dextran is 0.5% of that of the bismuth nitrate.
In the second step, 10mL of KCl solution, the number of moles of which is equal to that of bismuth nitrate, was added dropwise to the bismuth nitrate-glacial acetic acid solution. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 8 added dextran 20000, the dextran mole number being 0.5% of bismuth nitrate.
Fig. 9 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 8. As can be seen, in consideration of measurement errors, after the dextran 20000 assists the hydrothermal reaction, the BiOCl surface photovoltage signals have no obvious difference in the range of 300-400 nm.
Example 9:
, dissolving bismuth nitrate in glacial acetic acid, specifically, dissolving 5g of bismuth nitrate in 55mL of glacial acetic acid, and adding Sodium Dodecyl Benzene Sulfonate (SDBS), wherein the mole number of the SDBS is 5% of that of the bismuth nitrate.
In the second step, 10mL of KCl solution, the number of moles of which is equal to that of bismuth nitrate, was added dropwise to the bismuth nitrate-glacial acetic acid solution. Transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 180 ℃ for 24 hours, and naturally cooling to room temperature.
And thirdly, washing with deionized water and then with alcohol for 1-2 times, taking out the powder, dispersing the powder in the alcohol, drying at 80 ℃ to obtain a sample, and testing the surface photovoltage.
In contrast to comparative example 1, example 9 was run with SDBS, the SDBS mole being 5% of the bismuth nitrate.
Fig. 10 is a graph comparing surface photovoltage signals of the products obtained in comparative example 1 and example 9. As can be seen, after the addition of SDBS to assist the hydrothermal reaction, the BiOCl surface photovoltage signal is not enhanced in the range of 300-400 nm.
The above examples are only preferred embodiments of the patent, but the scope of protection of the patent is not limited thereto. It should be noted that, for those skilled in the art, without departing from the principle of this patent, several improvements and modifications can be made according to the patent solution and its patent idea, and these improvements and modifications should also be regarded as the protection scope of this patent.
Claims (3)
- The preparation method for remarkably enhancing BiOCl surface photovoltage signals is characterized by comprising the following steps:, dissolving bismuth nitrate in 40-60mL of glacial acetic acid, wherein the mass of bismuth nitrate/volume of glacial acetic acid =5g/40mL-5g/60mL, and then adding glucan to obtain a bismuth nitrate-glacial acetic acid-glucan solution, wherein the molar ratio of glucan to bismuth nitrate is 1-11%;the second step is that: dropwise adding a KCl solution into the bismuth nitrate-glacial acetic acid-glucan solution, transferring the generated precipitate into a hydrothermal reaction kettle, carrying out hydrothermal treatment at 160 ℃ and 180 ℃ for 24 hours, and naturally cooling to room temperature;the third step: washing the sample with deionized water, washing with alcohol for 1-2 times, taking out the powder, dispersing in alcohol, and drying at 60-80 deg.C to obtain the sample.
- 2. A method for preparing BiOCl with significantly enhanced surface photovoltage signal according to claim 1, which is characterized in that: the glucan is selected from glucan 20000.
- 3. A method for preparing BiOCl with significantly enhanced surface photovoltage signal according to claim 1, which is characterized in that: the BiOCl prepared by the method has obviously enhanced surface photovoltage signals in the range of 300-500 nm.
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| CN108816260A (en) * | 2018-05-16 | 2018-11-16 | 四川理工学院 | Surface photovoltage signal enhancing type (BiO)2CO3Preparation method |
| CN113457698B (en) * | 2021-06-16 | 2023-04-25 | 四川轻化工大学 | Method for improving BiOCl surface photovoltage signal |
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