CN114573025B - Preparation method and application of BiOCl and multiphase composite semiconductor material thereof - Google Patents
Preparation method and application of BiOCl and multiphase composite semiconductor material thereof Download PDFInfo
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- CN114573025B CN114573025B CN202210253253.4A CN202210253253A CN114573025B CN 114573025 B CN114573025 B CN 114573025B CN 202210253253 A CN202210253253 A CN 202210253253A CN 114573025 B CN114573025 B CN 114573025B
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- 239000000463 material Substances 0.000 title claims abstract description 114
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004065 semiconductor Substances 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 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 claims description 37
- 229940043267 rhodamine b Drugs 0.000 claims description 37
- 229910001414 potassium ion Inorganic materials 0.000 claims description 30
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000011941 photocatalyst Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 239000002033 PVDF binder Substances 0.000 claims description 9
- 238000002474 experimental method Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000006230 acetylene black Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000005286 illumination Methods 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 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 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- 229910001510 metal chloride Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002835 absorbance Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- MHEBVKPOSBNNAC-UHFFFAOYSA-N potassium;bis(fluorosulfonyl)azanide Chemical compound [K+].FS(=O)(=O)[N-]S(F)(=O)=O MHEBVKPOSBNNAC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000010345 tape casting Methods 0.000 claims description 2
- 238000012705 nitroxide-mediated radical polymerization Methods 0.000 claims 2
- 239000007773 negative electrode material Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 15
- 239000010410 layer Substances 0.000 description 9
- 239000010405 anode material Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- 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
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- B01J35/23—
-
- B01J35/39—
-
- B01J35/51—
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/582—Halogenides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
The application discloses a preparation method and application of BiOCl and a multiphase composite semiconductor material thereof. The BiOCl and the multiphase composite semiconductor material thereof prepared by the physical ball milling method have excellent electrochemical potassium storage performance and photocatalytic degradation performance of organic pollutants.
Description
Technical Field
The application belongs to the technical field of potassium ion batteries and photocatalytic degradation, and particularly relates to a preparation method and application of BiOCl and a multiphase composite semiconductor material thereof.
Background
In the background of the increasingly serious energy crisis and environmental crisis, how to efficiently treat environmental pollutants and develop new energy is a problem to be solved in the present day. The photocatalysis technology becomes one of the most effective methods for solving the environmental problems, and has the characteristics of low cost, quick response and no secondary pollution, and has attracted wide attention. In the early stages of photocatalytic research, the catalysts mainly involved were TiO 2 、CaTiO 3 Etc. However, these photocatalysts have low solar light utilization rate and high photo-generated electron-hole pair recombination rate, so that the photocatalysts have low photocatalytic activity. In order to overcome this problem, more and more researches are being conducted on photocatalysts, and photocatalysts with suitable band gaps and low photo-generated electron-hole recombination rate are sought to expand the light absorption range of the photocatalysts, so that high-efficiency photocatalytic activity is obtained.
BiOCl has attracted extensive attention from photocatalytic scientists due to its unique two-dimensional (2D) layered structure, electronic properties, optical properties and stability, non-toxicity, low cost, and a series of features. BiOCl is a typical layered structure material, has highly anisotropic electrical, mechanical and optical properties, and has wide application prospects. From Cl − And [ Bi ] 2 O 2 ] 2+ The stacking is formed, a built-in electric field is formed between the negative ion layer and the positive ion layer, which is favorable for effective separation of photo-generated electrons and holes, and BiOCl is an indirect band gap semiconductor which can effectively prevent recombination of the photo-generated electrons and holes, so that the photo-generated electrons and the positive ion layer show good photo-catalytic performance.
But the BiOCl material also has its own limitations, that is, no response to visible light, which is a major limiting factor in the practical application of photocatalytic degradation of pollutants. The modification of the BiOCl by utilizing metal ion doping and semiconductor coupling is an effective method for enlarging the BiOCl light absorption area and improving the charge separation efficiency. The metal ion doping is mainly carried out in a semiconductor main lattice, impurity energy levels can be generated in a band gap, and electron transition can be completed step by step, so that energy of a required light source is reduced, visible light photocatalysis is improved, semiconductor coupling is that different materials of semiconductors are coupled to form a heterojunction, difference exists between fermi energy levels of the heterojunction, energy band bending occurs on an interface of the semiconductor, an internal electric field is constructed, interface charge transfer is promoted, and visible light photocatalysis activity of the semiconductor is remarkably improved.
The BiOCl and the multiphase composite semiconductor material thereof have higher electrochemical activity, mechanical property and optical property, so that the BiOCl and the multiphase composite semiconductor material not only can be used in the field of photocatalysis, but also can be used for the cathode of a potassium ion battery. The lithium ion battery has taken up the main market in the energy storage field due to the characteristics of high energy density and long cycle life, but the development is limited by the problems of high price and limited reserve, so that the lithium ion battery commercialized at present is difficult to meet the requirement of large-scale energy storage, and the requirement of further exploring an energy storage system with low cost is required. The potassium ion battery is paid attention to because of abundant natural resources, low cost and similar working mechanism to the lithium ion battery. Is expected to become a substitute of lithium ion batteries, and is a promising energy storage system. At present, research on anode materials of potassium ion batteries is mainly focused on materials such as carbon-based materials, metal oxides, metal alloys and the like. But has a series of problems of lower capacity, quicker capacity attenuation, poor cycling stability, larger volume change in the charge and discharge process, and the like.
BiOCl is made of Cl − And [ Bi ] 2 O 2 ] 2+ The layered structure formed by stacking has the characteristics of strong intra-layer covalent bonds and weak inter-layer van der Waals interactions, can provide a rapid diffusion path between ion layers, and can provide larger volume expansion for potassium ion insertion and extractionExpansion. Because of the characteristics, researchers have focused on the novel metal halide material and applied BiOCl and the multiphase composite semiconductor material thereof to the anode material of the potassium ion battery. And the BiOCl and the multiphase composite semiconductor material thereof are low-cost, environment-friendly and easy-to-prepare compounds, and are very attractive green energy storage technology combined with a potassium ion battery.
Disclosure of Invention
The technical problems to be solved are as follows: in order to overcome the defects in the prior art, the application provides a preparation method and application of BiOCl and a multiphase composite semiconductor material thereof, which are used for solving the technical problems of low capacity, poor conductive performance, unstable cycle performance and the like of the existing potassium ion battery anode material in the prior art, expanding the light absorption range of a photocatalyst and obtaining higher efficient photocatalytic activity. The application provides a method for preparing BiOCl and a multiphase composite semiconductor material thereof, and the material can be applied to the fields of cathodes of potassium ion batteries and photocatalytic degradation of organic pollutants.
The technical scheme is as follows:
the raw materials of the BiOCl and the multiphase composite semiconductor material thereof are bismuth nitrate of 0.002-0.006 mol, 10% hydrochloric acid aqueous solution diluted by 2 mL, 3mL ultrapure water, 3mL absolute ethanol and metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony element of 0-0.004mol, and the single-phase BiOCl material or BiOCl-based multiphase composite semiconductor material is obtained through physical ball milling and centrifugation processes.
As a preferred technical scheme of the application: the preparation method comprises the following specific steps:
the first step: uniformly mixing 0.002-0.006 mol of bismuth nitrate, 2 mL diluted 10% hydrochloric acid aqueous solution, 3mL ultrapure water, 3mL of absolute ethyl alcohol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony elements by a physical ball milling method to obtain ball milling products;
and a second step of: and removing unreacted impurities in the ball-milling product through a centrifugal process to obtain a single-phase BiOCl material or a BiOCl-based multiphase composite material.
As a preferred technical scheme of the application: the physical ball milling method in the first step is that the ball milling rotating speed is 400-800 r min -1 Ball milling time is 0.5-6 h.
As a preferred technical scheme of the application: the centrifugal step in the second step is that the centrifugal rotation speed is 5000-10000 r min -1 Centrifuging for 10min, washing with deionized water for 3 times, collecting washed product, removing water solution and unreacted substances, oven drying, and grinding.
The application also discloses BiOCl and application of the multi-phase composite semiconductor material in photocatalytic degradation of organic pollutants.
As a preferred technical scheme of the application: performing photocatalytic degradation on rhodamine B (RhB) under a xenon lamp light source of 300W, weighing a single-phase BiOCl material or a multiphase composite semiconductor material thereof prepared by 0.05 g, adding the single-phase BiOCl material or the multiphase composite semiconductor material thereof into a beaker containing a RhB organic dye solution with the concentration of 150 mL of 10 ppm, putting the beaker into an ultrasonic cleaner for 5 min to uniformly disperse, putting the beaker on a magnetic stirrer, ensuring that the rotating speed can be kept at 600 rpm in the reaction process, and continuously and uniformly dispersing the single-phase BiOCl material or the multiphase composite semiconductor material thereof in the organic solution in the degradation process; before the photocatalytic degradation experiment is carried out, the prepared single-phase BiOCl material or the solution of the multiphase composite semiconductor material is placed in a dark condition for 30min for adsorption in a darkroom, so that the prepared single-phase BiOCl material or the multiphase composite semiconductor material and RhB reach adsorption-desorption balance; then turning on a light source to perform illumination experiment, sampling the simulated organic pollutant water solution every 5-10 min according to the photocatalytic degradation rates of different materials, taking 4 mL reaction solutions each time, and filtering out the photocatalyst by using an injection filter with the aperture of 0.22 mu m; the absorbance of the filtrate was analyzed by an ultraviolet-visible spectrophotometer at the maximum absorption wavelength 554, nm of RhB and converted to the corresponding concentration with reference to the RhB standard curve.
The application also discloses the BiOCl and the application of the multi-phase composite semiconductor material in the anode material of the potassium ion battery.
As a preferred technical scheme of the application: in the potassium ion battery assembly process, a BiOCl material or a multiphase composite semiconductor material thereof, acetylene black and PVDF (polyvinylidene fluoride) are mixed according to the mass ratio of 7:2:1 in NMP (N-methylpyrrolidone) and stirring for 6h; uniformly coating the mixture on a copper foil by using a doctor blade through a tape casting method; button cell battery loading operation is carried out in an argon atmosphere glove box, a counter electrode is a potassium sheet, a diaphragm is made of glass fiber materials, and electrolyte is 5 mol KFSI in DIGLYME solution.
As a preferred technical scheme of the application: the BiOCl material or the multiphase composite semiconductor material, the acetylene black and the PVDF material correspond to 0.5 mL NMP per 100 mg.
Principle explanation: biOCl materials or multiphase composite semiconductor materials thereof belong to a typical lamellar material, and a lamellar structure is formed by stacking intra-layer covalent bonds and interlayer van der Waals interactions, so that the material has higher electrochemical activity, mechanical property and optical property. And BiOCl is an indirect bandgap semiconductor that can effectively prevent recombination of photogenerated electrons and holes, and thus exhibits good photocatalytic performance. And the unique layered structure formed by interweaving the positive and negative ion layers can provide a rapid diffusion path along and between the ion layers and the layered structure unit can provide larger volume expansion for the insertion and extraction of potassium ions. Such materials can be applied in potassium ion batteries and exhibit superior electrochemical performance.
The beneficial effects are that:
1. the BiOCl material is an indirect band gap semiconductor and has good photocatalytic performance in the process of photocatalytic degradation of RhB.
2. The BiOCl material provided by the application has the advantages of good conductivity, high specific capacity and good cycling stability, and is used as a negative electrode of a potassium ion battery, and excellent electrochemical potassium storage performance is shown.
3. Compared with the BiOCl material, the BiOCl multiphase composite semiconductor material has the advantages of remarkably improved photocatalytic performance, high initial coulomb efficiency, smaller irreversible capacity and better cycle stability.
4. The preparation method of the application has the advantages of simplicity, short period, easily available raw materials, low cost and huge industrialization application value.
5. The material of the application has wider application field, is not only limited to the anode material of the potassium ion battery, but also can be applied to the field of photocatalytic degradation of organic pollutants, and has better application prospect.
6. The BiOCl material prepared by the ball milling method is used for photocatalytic degradation of rhodamine B (RhB), and basically degraded in 60 minutes under the illumination condition, so that the BiOCl material has excellent photocatalytic performance.
7. BiOCl material prepared by ball milling method is used as anode material of potassium ion battery, and is 0.1: 0.1A g -1 The specific charge capacity after 200 cycles is kept at 363mAh g -1 Exhibit a higher specific capacity and excellent cycle stability.
8. BiOCl/Amorphos-Sb prepared by ball milling method 2 O 3 The (BOC/AAO) material is used for photocatalytic degradation of rhodamine B (RhB), and the rhodamine B is basically degraded in 20 minutes under the illumination condition, so that the photocatalytic performance of the rhodamine B is obviously improved compared with that of single-phase BiOCl.
9. BOC/AAO material prepared by ball milling method as anode material of potassium ion battery, in 0.1A g -1 The first-turn coulombic efficiency was 57.2% and the specific charge capacity after 200 turns of the cycle remained at 328mAh g -1 Compared with single-phase BiOCl, the first-circle coulomb efficiency is improved, the irreversible capacity is reduced, and the cycle stability is excellent.
Drawings
FIG. 1 is an XRD pattern for BiOCl materials made in accordance with the present application.
FIG. 2 is an SEM image of a BiOCl material made in accordance with the present application.
FIG. 3 is a graph showing the relationship of photocatalytic degradation of RhB by BiOCl material prepared by the present application.
Fig. 4 is a charge-discharge graph of the BiOCl material prepared according to the present application as a negative electrode of a potassium ion battery.
FIG. 5 is a graph showing the long cycle performance of the BiOCl material prepared in accordance with the present application as a negative electrode of a potassium ion battery.
FIG. 6 is a graph showing the relationship of photocatalytic degradation of RhB by the BOC/AAO material prepared by the present application.
FIG. 7 is a graph showing charge and discharge of BOC/AAO materials prepared according to the present application as a negative electrode of a potassium ion battery.
FIG. 8 is a graph showing the long cycle performance of the BOC/AAO material prepared according to the present application as a negative electrode of a potassium ion battery.
Detailed Description
The technical solution of the present application will be further described with reference to the drawings and specific examples, which are only for illustrating the present application, and the present application is not limited to the following examples. All modifications and equivalent substitutions to the technical proposal of the application are included in the protection scope of the application without departing from the spirit and scope of the technical proposal of the application.
In the following examples, the raw materials were 0.002-0.006 mol bismuth nitrate, 2 mL diluted 10% hydrochloric acid aqueous solution, 3mL ultrapure water, 3mL absolute ethanol, and 0-0.004mol metal chlorides of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium, or antimony, and single-phase BiOCl materials or BiOCl-based multiphase composite semiconductor materials were obtained by physical ball milling and centrifugation processes. The material is used for manufacturing a cathode of a potassium ion battery for electrochemical test and for carrying out related test of photocatalytic degradation of RhB.
Example 1:
a preparation method of the BiOCl material comprises the following steps:
the first step: 0.006 mol of Bi (NO) was weighed out 3 ) 3 ·5H 2 Adding O into an agate ball milling tank; then adding 2 mL diluted 10% hydrochloric acid aqueous solution, 3mL water and 3mL absolute ethanol in sequence; setting the ball milling rotating speed to be 500 r min -1 Ball milling time is 0.5 h;
and a second step of: collecting ball-milled products in a centrifuge tube, and setting the centrifugal rotating speed to 8000 r min -1 The centrifugation time is 10min, washing is carried out 3 times by deionized water, and the washing is collected in the centrifugation processAnd removing the aqueous solution and unreacted substances from the obtained product, and drying and grinding to obtain the BiOCl material.
XRD characterization of BiOCl material is shown in figure 1, and microscopic morphology is shown in figure 2, and it can be seen that the diffraction peaks of the synthesized material correspond to diffraction peaks in a standard BiOCl PDF card one by one. And the BiOCl mainly comprises nano sheets, the nano sheets have uniform thickness, and the layers are closely and regularly stacked to form a flower ball-like shape.
The material prepared in this example was tested for photocatalytic degradation of the organic dye rhodamine B (RhB).
Photocatalytic degradation of rhodamine B (RhB): performing photocatalytic degradation on rhodamine B (RhB) under a xenon lamp light source of 300W, weighing a single-phase BiOCl material prepared by 0.05 g, adding the single-phase BiOCl material into a beaker containing a RhB organic dye solution with the concentration of 150 mL of 10 ppm, putting the beaker into an ultrasonic cleaner, performing ultrasonic treatment for 5 min to perform uniform dispersion, putting the beaker on a magnetic stirrer, ensuring that the rotating speed can be kept at 600 rpm in the reaction process, and continuously and uniformly dispersing the BiOCl material in the organic solution in the degradation process; before the photocatalytic degradation experiment is carried out, the solution added with BiOCl is firstly placed under the dark condition for 30min of darkroom adsorption, so that the BiOCl and RhB reach adsorption-desorption equilibrium; then turning on a light source to perform illumination experiment, sampling the simulated organic pollutant water solution every 10min, taking 4 mL reaction solutions each time, and filtering out the photocatalyst by using an injection filter with the aperture of 0.22 mu m; the absorbance of the filtrate was analyzed by an ultraviolet-visible spectrophotometer at the maximum absorption wavelength 554, nm of RhB and converted to the corresponding concentration with reference to the RhB standard curve.
The photocatalytic degradation relationship curve of the BiOCl material for photocatalytic degradation of RhB is shown in FIG. 3.
The material prepared in the embodiment is used as a raw material to assemble a potassium ion battery, and the battery performance is tested.
And (3) assembling a potassium ion battery: the preparation method comprises the following steps of (1) mixing BiOCl, acetylene black and PVDF (polyvinylidene fluoride) according to a mass ratio of 7:2:1 in NMP (N-methyl pyrrolidone) for 6h; the BiOCl, acetylene black, PVDF material corresponds to 0.5 mL NMP per 100 mg. The mixture was uniformly coated on a copper foil using a doctor blade by a casting method. Button cell battery loading operation is carried out in an argon atmosphere glove box, a counter electrode is a potassium sheet, a diaphragm is made of glass fiber materials, and electrolyte is 5 mol KFSI in DIGLYME solution.
The assembled potassium ion battery was subjected to a battery performance test, the test results are shown in fig. 4-5.
Example 2:
a preparation method of a BiOCl multiphase composite semiconductor material comprises the following steps:
the first step: 0.003 mol of Bi (NO) was weighed out according to the molecular formula 3 ) 3 ·5H 2 O and 0.003 mol SbCl 3 Added to an agate ball milling pot. Then 10% aqueous hydrochloric acid diluted with 2 mL, 3mL water, 3mL absolute ethanol were added sequentially. Setting the ball milling rotating speed to be 500 r min -1 Ball milling time is 2 h;
and a second step of: collecting ball-milled products in a centrifuge tube, and setting the centrifugal speed to 10000 r min -1 And (3) washing 3 times with deionized water for 10min, collecting the washed product in the centrifugation process, removing the aqueous solution and unreacted substances, and drying and grinding to obtain the BiOCl multiphase composite semiconductor material.
The material prepared in this example was tested for photocatalytic degradation of the organic dye rhodamine B (RhB).
Photocatalytic degradation of rhodamine B (RhB): all experiments were performed under a 300W xenon lamp light source. The BOC/AAO material prepared by weighing 0.05 and g is added into a beaker containing a RhB organic dye solution with the concentration of 150 mL being 10 ppm, and is put into an ultrasonic cleaner for ultrasonic treatment for 5 min to be uniformly dispersed, and the beaker is placed on a magnetic stirrer to ensure that the rotating speed can be kept at 600 rpm in the reaction process, so that the BOC/AAO is continuously and uniformly dispersed in the organic solution in the degradation process. Before the photocatalytic degradation experiment is carried out, the solution added with BOC/AAO is firstly placed under the dark condition for 30min in a darkroom for adsorption, so that the BOC/AAO and RhB reach adsorption-desorption balance. Then, the light source was turned on to perform an illumination experiment, the aqueous solution of the simulated organic pollutant was sampled every 5 minutes, 4 mL reaction solutions were taken each time, and the photocatalyst was filtered out with a syringe filter having a pore size of 0.22 μm. The absorbance of the filtrate was analyzed by an ultraviolet-visible spectrophotometer at the maximum absorption wavelength 554, nm of RhB and converted to the corresponding concentration with reference to the RhB standard curve.
The photocatalytic degradation relationship curve of the photocatalytic degradation of the BOC/AAO material for RhB is shown in FIG. 6.
The material prepared in the embodiment is used as a raw material to assemble a potassium ion battery, and the battery performance is tested.
And (3) assembling a potassium ion battery: BOC/AAO, acetylene black and PVDF (polyvinylidene fluoride) are mixed according to the mass ratio of 7:2:1 in NMP (N-methyl pyrrolidone) for 6h; the BOC/AAO, acetylene black, PVDF material corresponds to 0.5 mL NMP per 100 mg. The mixture was uniformly coated on a copper foil using a doctor blade by a casting method. Button cell battery loading operation is carried out in an argon atmosphere glove box, a counter electrode is a potassium sheet, a diaphragm is made of glass fiber materials, and electrolyte is 5 mol KFSI in DIGLYME solution.
The assembled potassium ion battery was subjected to battery performance testing, the test results are shown in fig. 7-8.
Example 3:
a preparation method of BiOCl and a multiphase composite semiconductor material thereof comprises the following steps:
the first step: 0.003 mol of Bi (NO) was weighed out according to the molecular formula 3 ) 3 ·5H 2 O and 0.003 mol FeCl 3 Added to an agate ball milling pot. Then 10% aqueous hydrochloric acid diluted with 2 mL, 3mL water, 3mL absolute ethanol were added sequentially. Setting the ball milling rotating speed to 700 r min -1 Ball milling time is 5 h;
and a second step of: collecting ball-milled products in a centrifuge tube, and setting the centrifugal speed to 10000 r min -1 The centrifugation time is 10min, washing is carried out 3 times by deionized water, the washed product is collected in the centrifugation process, the aqueous solution and unreacted substances are removed, and the product is dried and ground.
Example 4:
a preparation method of BiOCl and a multiphase composite semiconductor material thereof comprises the following steps:
the first step: weighing 0.002 mol of Bi (NO) 3 ) 3 ·5H 2 O and 0.004mol of CoCl 2 ·6H 2 O was added to an agate ball milling pot. Then sequentially adding 2mL of diluted 10% aqueous hydrochloric acid, 3mL water, 3mL absolute ethanol. Setting the ball milling rotating speed to be 500 r min -1 Ball milling time is 5 h;
and a second step of: collecting ball-milled products in a centrifuge tube, and setting the centrifugal speed to 10000 r min -1 The centrifugation time is 10min, washing is carried out 3 times by deionized water, the washed product is collected in the centrifugation process, the aqueous solution and unreacted substances are removed, and the product is dried and ground.
Example 5:
a preparation method of BiOCl and a multiphase composite semiconductor material thereof comprises the following steps:
the first step: 0.004mol of Bi (NO) is weighed according to the molecular formula 3 ) 3 ·5H 2 O and 0.002 mol of NiCl 2 ·6H 2 O was added to an agate ball milling pot. Then 10% aqueous hydrochloric acid diluted with 2 mL, 3mL water, 3mL absolute ethanol were added sequentially. Setting the ball milling rotating speed to 600 r min -1 Ball milling time is 3 h;
and a second step of: collecting ball-milled products in a centrifuge tube, and setting the centrifugal rotating speed to 9000 r min -1 The centrifugation time is 10min, washing is carried out 3 times by deionized water, the washed product is collected in the centrifugation process, the aqueous solution and unreacted substances are removed, and the product is dried and ground.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. A preparation method of BiOCl and a multiphase composite semiconductor material thereof is characterized in that: the BiOCl and the multiphase composite semiconductor material thereof are prepared from 0.002-0.006 mol of bismuth nitrate, 2 mL diluted 10% hydrochloric acid aqueous solution, 3mL ultrapure water, 3mL of absolute ethyl alcohol and 0-0.004mol of metal chlorides of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony, and the single-phase BiOCl material or the BiOCl-based multiphase composite semiconductor material is obtained through physical ball milling and centrifugation processes, and the specific steps are as follows:
the first step: uniformly mixing 0.002-0.006 mol of bismuth nitrate, 2 mL diluted 10% hydrochloric acid aqueous solution, 3mL ultrapure water, 3mL of absolute ethyl alcohol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony elements by a physical ball milling method to obtain ball milling products; the physical ball milling method is that the ball milling rotating speed is 400-800 r min -1 Ball milling time is 0.5-6 h;
and a second step of: and removing unreacted impurities in the ball-milling product through a centrifugal process to obtain a single-phase BiOCl material or a BiOCl-based multiphase composite material.
2. The method for preparing the BiOCl and the multiphase composite semiconductor material thereof according to claim 1, which is characterized in that: the centrifugal step in the second step is that the centrifugal rotation speed is 5000-10000 r min -1 Centrifuging for 10min, washing with deionized water for 3 times, collecting washed product, removing water solution and unreacted substances, oven drying, and grinding.
3. Use of BiOCl and its heterogeneous composite semiconductor material prepared by the preparation method of claim 1 in photocatalytic degradation of organic pollutants.
4. The use of BiOCl and its heterogeneous composite semiconductor material in a negative electrode material for a potassium ion battery prepared by the preparation method of claim 1.
5. A use according to claim 3, characterized in that: performing photocatalytic degradation on rhodamine B RhB under a xenon lamp light source of 300W, weighing a single-phase BiOCl material or a multiphase composite semiconductor material thereof prepared by 0.05 g, adding the single-phase BiOCl material or the multiphase composite semiconductor material thereof into a beaker containing a RhB organic dye solution with the concentration of 150 mL of 10 ppm, putting the beaker into an ultrasonic cleaner for 5 min to uniformly disperse, putting the beaker on a magnetic stirrer, ensuring that the rotating speed can be kept at 600 rpm in the reaction process, and continuously and uniformly dispersing the single-phase BiOCl material or the multiphase composite semiconductor material thereof in the organic solution in the degradation process; before the photocatalytic degradation experiment is carried out, the prepared single-phase BiOCl material or the solution of the multiphase composite semiconductor material is placed in a dark condition for 30min for adsorption in a darkroom, so that the prepared single-phase BiOCl material or the multiphase composite semiconductor material and RhB reach adsorption-desorption balance; then turning on a light source to perform illumination experiment, sampling the simulated organic pollutant water solution every 5-10 min according to the photocatalytic degradation rates of different materials, taking 4 mL reaction solutions each time, and filtering out the photocatalyst by using an injection filter with the aperture of 0.22 mu m; the absorbance of the filtrate was analyzed by an ultraviolet-visible spectrophotometer at the maximum absorption wavelength 554, nm of RhB and converted to the corresponding concentration with reference to the RhB standard curve.
6. The use according to claim 4, characterized in that: in the potassium ion battery assembly process, a BiOCl material or a multiphase composite semiconductor material thereof, acetylene black and PVDF polyvinylidene fluoride are mixed according to the mass ratio of 7:2:1 in N-methyl pyrrolidone NMP, mixing and stirring 6h; uniformly coating the mixture on a copper foil by using a doctor blade through a tape casting method; button cell battery loading operation is carried out in an argon atmosphere glove box, a counter electrode is a potassium sheet, a diaphragm is made of glass fiber materials, and electrolyte is 5 mol KFSI in DIGLYME solution.
7. The use according to claim 6, characterized in that: the BiOCl material or the multiphase composite semiconductor material, the acetylene black and the PVDF material correspond to 0.5 mL NMP per 100 mg.
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