CN114573025A - BiOCl and preparation method and application of multiphase composite semiconductor material thereof - Google Patents
BiOCl and preparation method and application of multiphase composite semiconductor material thereof Download PDFInfo
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- CN114573025A CN114573025A CN202210253253.4A CN202210253253A CN114573025A CN 114573025 A CN114573025 A CN 114573025A CN 202210253253 A CN202210253253 A CN 202210253253A CN 114573025 A CN114573025 A CN 114573025A
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- 239000000463 material Substances 0.000 title claims abstract description 118
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000004065 semiconductor Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims description 12
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052802 copper Inorganic materials 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052738 indium Inorganic materials 0.000 claims abstract description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 239000011777 magnesium Substances 0.000 claims abstract description 6
- 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 abstract description 6
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 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
- 239000010936 titanium Substances 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 6
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 238000006731 degradation reaction Methods 0.000 claims abstract description 5
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 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 44
- 229940043267 rhodamine b Drugs 0.000 claims description 44
- 229910001414 potassium ion Inorganic materials 0.000 claims description 33
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 31
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 12
- 239000011941 photocatalyst Substances 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 239000006230 acetylene black Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000000227 grinding 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
- 238000005406 washing Methods 0.000 claims description 7
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 5
- 238000002835 absorbance Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 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
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 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
- 238000010345 tape casting Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning 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
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 239000011148 porous material 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
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 18
- 239000000126 substance Substances 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000000593 degrading effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000031700 light absorption Effects 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
- 239000010406 cathode material Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process 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
- 238000000605 extraction Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process 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
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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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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- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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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
- 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
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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
- 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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Abstract
The material is prepared by taking bismuth nitrate, metal chlorides of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium and antimony elements, hydrochloric acid, ultrapure water and ethanol as raw materials through a physical ball milling method, collecting a precipitation product through a centrifugal process, and removing an aqueous solution and unreacted substances in the aqueous solution to obtain a single-phase BiOCl material or a BiOCl-based multiphase composite material. The BiOCl and the multiphase composite semiconductor material thereof prepared by the physical ball milling method have excellent electrochemical potassium storage performance and photocatalytic organic pollutant degradation performance.
Description
Technical Field
The invention 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
Under the background that the energy crisis and the environmental crisis are becoming more serious, how to efficiently treat environmental pollutants and develop new energy become the problems which need to be solved urgently nowadays. The photocatalytic technology becomes one of the most effective methods for solving the environmental problems, and the photocatalytic degradation of organic pollutants 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 catalyst mainly involved was TiO2、CaTiO3And the like. However, the photocatalysts have low utilization rate to sunlight and high recombination rate of photo-generated electron-hole pairs, so that the photocatalysts have low activity. In order to overcome the problem, people have conducted more and more researches on the photocatalyst, and have searched for a photocatalyst with a suitable band gap and a low recombination rate of photo-generated electron holes so as to expand the light absorption range of the photocatalyst, thereby obtaining high-efficiency photocatalytic activity.
BiOCl has attracted extensive attention of photocatalytic scientists due to its unique two-dimensional (2D) layered structure, electronic properties, optical properties and stability, as well as a series of characteristics of non-toxicity, low price, and the like. BiOCl is a typical layered structure material, has highly anisotropic electrical, mechanical and optical properties, and has wide application prospects. From Cl−And [ Bi ]2O2]2+Stack formation with built-in electric field between its negative and positive ion layers facilitates efficient separation of photo-generated electrons-holes, and BiOCl is a speciesThe indirect bandgap semiconductor can effectively prevent the recombination of photogenerated electrons and holes, and thus exhibits good photocatalytic performance.
However, the BiOCl material has its own limitations, and it is not responsive to visible light, which is a major limiting factor in its practical application to photocatalytic degradation of pollutants. The method for modifying the BiOCl light absorption area by using 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 body lattice, impurity energy levels can be generated in a band gap, and the transition of electrons can be completed step by step, so that the energy of a required light source is reduced, the visible light photocatalysis is improved, the semiconductor coupling is that semiconductors of different materials are coupled to form a heterojunction, the Fermi energy levels of the heterojunction are different, the energy band bending is generated on the interface of the semiconductor, an internal electric field is constructed, the interface charge transfer is promoted, and the visible light photocatalysis activity of the heterojunction is obviously improved.
BiOCl and its multiphase composite semiconductor material have high electrochemical activity, mechanical property and optical property, so that it can be used not only in the field of photocatalysis, but also in the negative pole of potassium ion battery. The lithium ion battery occupies the main market of the energy storage field due to the characteristics of high energy density and long cycle life, but the development of the lithium ion battery is limited due to the problems of high price and limited storage capacity, so that the current commercialized lithium ion battery is difficult to meet the requirement of large-scale energy storage, and further exploration of a low-cost energy storage system is required. Potassium ion batteries are of great interest because of their abundant natural resources, low cost, and similar working mechanism to lithium ion batteries. Is expected to become a substitute of a lithium ion battery and is a promising energy storage system. Currently, research on the anode material of the potassium ion battery is mainly focused on carbon-based materials, metal oxides, metal alloys and other materials. But has a series of problems of low capacity, fast capacity attenuation, poor cycle stability, large volume change in the charging and discharging process and the like.
BiOCl is Cl−And [ Bi ]2O2]2+Stacked to form a layered structure having layers thereinThe structure not only can provide a rapid diffusion path between the ion layer and the ion layer, but also can provide larger volume expansion for the insertion and extraction of potassium ions. Due to the characteristics, researchers put their attention on the novel metal halide material and apply BiOCl and the multiphase composite semiconductor material thereof to the negative electrode material of the potassium ion battery. And BiOCl and the multiphase composite semiconductor material thereof are compounds which are low in price, friendly to environment and easy to prepare, and are combined with a potassium ion battery to be very attractive green energy storage technology.
Disclosure of Invention
The technical problem to be solved is 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, so as to solve the technical problems of low capacity, poor conductivity, unstable cycle performance and the like of the conventional potassium ion battery cathode material in the prior art, expand the light absorption range of a photocatalyst and obtain high-efficiency photocatalytic activity. The invention provides a method for preparing BiOCl and a multiphase composite semiconductor material thereof, and the material can be applied to the negative electrode of a potassium ion battery and the field of photocatalytic degradation of organic pollutants.
The technical scheme is as follows:
the raw materials of BiOCl and the multiphase composite semiconductor material thereof are 0.002-0.006 mol of bismuth nitrate, 2 mL of diluted 10% hydrochloric acid aqueous solution, 3mL of ultrapure water, 3mL of anhydrous ethanol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony element, and the single-phase BiOCl material or the BiOCl-based multiphase composite semiconductor material is obtained through physical ball milling and a centrifugal process.
As a preferred technical scheme of the application: the preparation method comprises the following specific steps:
the first step is as follows: uniformly mixing 0.002-0.006 mol of bismuth nitrate, 2 mL of diluted 10% hydrochloric acid aqueous solution, 3mL of ultrapure water, 3mL of anhydrous ethanol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony element by using a physical ball milling method to obtain a ball-milled product;
the second step is that: and removing unreacted impurities in the obtained ball-milling product through a centrifugal process to obtain the single-phase BiOCl material or the 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--1And the ball milling time is 0.5-6 h.
As a preferred technical scheme of the application: the centrifugation step in the second step is that the centrifugation rotating speed is 5000-10000 r min-1Centrifuging for 10min, washing with deionized water for 3 times, collecting washed product, removing water solution and unreacted material, oven drying, and grinding.
The application also discloses application of the BiOCl and the multiphase composite semiconductor material thereof in degrading organic pollutants under photocatalysis.
As a preferred technical scheme of this application: carrying out photocatalytic degradation on rhodamine B (RhB) under a 300W xenon lamp light source, weighing 0.05 g of prepared single-phase BiOCl material or multi-phase composite semiconductor material thereof, adding the single-phase BiOCl material or the multi-phase composite semiconductor material thereof into a beaker containing 150 mL of 10 ppm RhB organic dye solution, putting the beaker into an ultrasonic cleaning machine, carrying out ultrasonic treatment for 5 min to carry out uniform dispersion, placing the beaker on a magnetic stirrer, and ensuring that the rotating speed can be kept at 600 rpm in the reaction process so that the prepared single-phase BiOCl material or the multi-phase composite semiconductor material thereof is continuously and uniformly dispersed in the organic solution in the degradation process; before a photocatalytic degradation experiment is carried out, a prepared solution of the single-phase BiOCl material or the multi-phase composite semiconductor material thereof needs to be placed in a dark condition for 30min in a dark room for adsorption, so that the prepared single-phase BiOCl material or the multi-phase composite semiconductor material thereof and RhB reach adsorption-desorption balance; then turning on a light source to carry out an illumination experiment, sampling the simulated organic pollutant aqueous solution every 5-10 min according to the photocatalytic degradation rate of different materials, taking 4 mL of reaction solution each time, and filtering out the photocatalyst by using an injection filter with the pore diameter of 0.22 mu m; the absorbance of the filtrate was analyzed using an ultraviolet-visible spectrophotometer at a RhB maximum absorption wavelength of 554 nm, and converted to the corresponding concentration with reference to a RhB standard curve.
The application also discloses application of the BiOCl and the multiphase composite semiconductor material thereof in a potassium ion battery cathode material.
As a preferred technical scheme of the application: in the assembling process of the potassium ion battery, the BiOCl material or the 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-methyl pyrrolidone) for 6 hours; uniformly coating the mixture on a copper foil by using a scraper through a tape casting method; and (3) carrying out button cell installation operation in an argon atmosphere glove box, wherein the counter electrode is a potassium sheet, the diaphragm is made of glass fiber, and the electrolyte is 5 mol of KFSI in DIGLYME solution.
As a preferred technical scheme of the application: the BiOCl material or the multiphase composite semiconductor material thereof, the acetylene black and the PVDF material correspond to 0.5 mL of NMP per 100 mg.
Principle explanation: BiOCl material or its multiphase composite semiconductor material belongs to a typical layered material, its layered structure is formed by stacking of intralayer covalent bond and interlayer Van der Waals interaction, and has high electrochemical activity, mechanical property and optical property. And BiOCl is an indirect bandgap semiconductor that can effectively prevent the recombination of photo-generated electrons and holes, and thus exhibits good photocatalytic performance. And the unique laminated structure formed by interweaving the positive ion layer and the negative ion layer can provide a rapid diffusion path between the ion layers and along the ion layers, and the laminated structure unit can provide large volume expansion for the insertion and extraction of potassium ions. It can be applied to a potassium ion battery and exhibits superior electrochemical properties.
Has the advantages that:
1. the BiOCl material is an indirect band gap semiconductor, and shows good photocatalytic performance in the process of photocatalytic degradation of RhB.
2. The BiOCl material disclosed by the invention is good in conductivity, high in specific capacity and good in cycling stability, and shows excellent electrochemical potassium storage performance when being used as a potassium ion battery cathode.
3. The BiOCl multiphase composite semiconductor material provided by the invention has the advantages that the photocatalytic performance is obviously improved, and compared with the BiOCl material, the BiOCl multiphase composite semiconductor material serving as a potassium ion battery cathode has the advantages of high coulombic efficiency of the first loop, smaller irreversible capacity and better cycling stability.
4. The method has the advantages of simple preparation method, short period, easily obtained raw materials, low cost and great industrial application value.
5. The material disclosed by the invention has wider application field, is not only limited to the cathode material of a 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 degrading rhodamine B (RhB) in a photocatalytic manner, basically degrading the rhodamine B (RhB) within 60 min under the illumination condition, and showing excellent photocatalytic performance.
7. The BiOCl material prepared by the ball milling method is used as the negative electrode material of the potassium ion battery and is 0.1A g-1The charging specific capacity is kept to 363mAh g after 200 cycles of circulation under the current density-1And the high specific capacity and excellent cycling stability are shown.
8. BiOCl/Amorphous-Sb prepared by ball milling2O3The (BOC/AAO) material is used for degrading rhodamine B (RhB) in a photocatalytic manner, basically degrading the rhodamine B (RhB) within 20 min under the illumination condition, and compared with single-phase BiOCl, the photocatalytic performance of the material is obviously improved.
9. The BOC/AAO material prepared by the ball milling method is used as the negative electrode material of the potassium ion battery and is 0.1A g-1The coulombic efficiency of the first turn is 57.2%, and the charging specific capacity is kept to be 328mAh g after 200 cycles of circulation-1Compared with single-phase BiOCl, the first-turn coulombic efficiency is improved, the irreversible capacity is reduced, and the cycle stability is excellent.
Drawings
Figure 1 is an XRD pattern of the BiOCl material made herein.
FIG. 2 is an SEM image of a BiOCl material made herein.
FIG. 3 is a graph showing the relationship between photocatalytic degradation of BiOCl material prepared by the present application and photocatalytic degradation of RhB.
Fig. 4 is a charge-discharge curve diagram of the BiOCl material prepared by the method as a potassium ion battery cathode.
FIG. 5 is a long cycle performance graph of the BiOCl material prepared by the method as a potassium ion battery cathode.
FIG. 6 is a graph showing the relationship between the photocatalytic degradation of RhB in the BOC/AAO material prepared by the present application.
FIG. 7 is a charge-discharge curve diagram of the BOC/AAO material prepared by the present application as a negative electrode of a potassium ion battery.
FIG. 8 is a graph of the long cycle performance of the BOC/AAO material prepared in the present application as a negative electrode of a potassium ion battery.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and specific examples, which are only used for illustrating the present invention and are not limited to the following examples. It is intended to cover by the present invention all such modifications as come within the scope of the invention as defined by the appended claims.
In the following examples, the raw materials were 0.002 to 0.006 mol of bismuth nitrate, 2 mL of diluted 10% aqueous hydrochloric acid, 3mL of ultrapure water, 3mL of anhydrous ethanol, and 0 to 0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium, or antimony, and a single-phase BiOCl material or a BiOCl-based multiphase composite semiconductor material was obtained by physical ball milling and centrifugation. The material is used for manufacturing a potassium ion battery cathode for electrochemical test and is used for carrying out related test of photocatalytic degradation RhB.
Example 1:
a preparation method of BiOCl material comprises the following steps:
the first step is as follows: weighing 0.006 mol of Bi (NO)3)3·5H2Adding O into an agate ball milling tank; then sequentially adding 2 mL of diluted 10% hydrochloric acid aqueous solution, 3mL of water and 3mL of absolute ethyl alcohol; setting the ball milling speed at 500 rpm-1Ball, ballThe grinding time is 0.5 h;
the second step is that: collecting ball-milled product in a centrifuge tube, setting the centrifuge speed at 8000 r min-1And (3) centrifuging for 10min, washing for 3 times by using deionized water, collecting a washed product in the centrifuging process, removing the aqueous solution and unreacted substances, drying and grinding to obtain the BiOCl material.
The XRD characterization of the BiOCl material is shown in the attached figure 1, the microstructure is shown in the figure 2, and the diffraction peaks of the synthesized material correspond to the 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 are closely and regularly stacked to form a shape similar to a flower ball.
The material prepared in the embodiment is used for testing photocatalytic degradation of organic dye rhodamine B (RhB).
Photocatalytic degradation of rhodamine B (RhB): carrying out photocatalytic degradation on rhodamine B (RhB) under a 300W xenon lamp light source, weighing 0.05 g of prepared single-phase BiOCl material, adding the single-phase BiOCl material into a beaker containing 150 mL of RhB organic dye solution with the concentration of 10 ppm, putting the beaker into an ultrasonic cleaning machine, carrying out ultrasonic treatment for 5 min to carry out uniform dispersion, placing the beaker on a magnetic stirrer, and ensuring that the rotating speed can be kept at 600 rpm in the reaction process so that the BiOCl material is continuously and uniformly dispersed in the organic solution in the degradation process; before carrying out a photocatalytic degradation experiment, a solution added with BiOCl is required to be placed in a dark condition for 30min in a dark room for adsorption, so that the adsorption-desorption balance between the BiOCl and the RhB is achieved; then turning on a light source to carry out an illumination experiment, sampling the simulated organic pollutant aqueous solution every 10min, taking 4 mL of reaction solution every 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 using an ultraviolet-visible spectrophotometer at a RhB maximum absorption wavelength of 554 nm, and converted to the corresponding concentration with reference to a RhB standard curve.
The photocatalytic degradation relation curve of the BiOCl material for photocatalytic degradation of RhB is shown in figure 3.
The material prepared in the embodiment is used as a raw material to assemble a potassium ion battery, and the performance of the battery is tested.
Assembling the potassium ion battery: adding BiOCl, acetylene black and PVDF (polyvinylidene fluoride) according to a mass ratio of 7: 2: 1 in NMP (N-methyl pyrrolidone) for 6 hours; and each 100 mg of the BiOCl, acetylene black and PVDF materials corresponds to 0.5 mL of NMP. The mixture was uniformly coated on a copper foil by a doctor blade using a tape casting method. And (3) carrying out button cell assembly operation in an argon atmosphere glove box, wherein the counter electrode is a potassium sheet, the diaphragm is made of glass fiber, and the electrolyte is 5 mol of KFSI in DIGLYME solution.
The assembled potassium ion battery was subjected to battery performance tests, the test results being shown in fig. 4-5.
Example 2:
a preparation method of a BiOCl multiphase composite semiconductor material comprises the following steps:
the first step is as follows: weighing 0.003 mol of Bi (NO) according to the molecular formula3)3·5H2O and 0.003 mol of SbCl3Adding into an agate ball milling tank. Then 2 mL of diluted 10% aqueous hydrochloric acid, 3mL of water, and 3mL of absolute ethanol were added in this order. Setting the ball milling speed at 500 rpm-1The ball milling time is 2 h;
the second step is that: collecting ball-milled products in a centrifuge tube, and setting the centrifuge speed to 10000 r min-1And (3) washing with deionized water for 3 times for 10min, collecting a washed product in the centrifugation process, removing the aqueous solution and unreacted substances, drying and grinding to obtain the BiOCl multiphase composite semiconductor material.
The material prepared in the embodiment is used for testing photocatalytic degradation of organic dye rhodamine B (RhB).
Photocatalytic degradation of rhodamine B (RhB): all experiments were performed under a 300W xenon lamp light source. Weighing 0.05 g of the prepared BOC/AAO material, adding the BOC/AAO material into a beaker filled with 150 mL of 10 ppm RhB organic dye solution, putting the beaker into an ultrasonic cleaning machine for ultrasonic treatment for 5 min for uniform dispersion, and placing the beaker 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 material is continuously and uniformly dispersed in the organic solution in the degradation process. Before the photocatalytic degradation experiment, the solution added with the BOC/AAO is placed in the dark for 30min in a dark room for adsorption, so that the adsorption-desorption balance between the BOC/AAO and the RhB is achieved. Then, the light source was turned on to perform the light experiment, the aqueous solution of the simulated organic contaminants was sampled every 5 min, 4 mL of the reaction solution was taken each time, and the photocatalyst was filtered off with a syringe filter having a pore size of 0.22. mu.m. The absorbance of the filtrate was analyzed using an ultraviolet-visible spectrophotometer at a RhB maximum absorption wavelength of 554 nm, and converted to the corresponding concentration with reference to a RhB standard curve.
The photocatalytic degradation relation curve of the BOC/AAO material for photocatalytic degradation of 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 performance of the battery is tested.
Assembling the 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 6 hours; the BOC/AAO, the acetylene black and the PVDF material correspond to 0.5 mL of NMP per 100 mg. The mixture was uniformly coated on a copper foil by a doctor blade using a tape casting method. And (3) carrying out button cell assembly operation in an argon atmosphere glove box, wherein the counter electrode is a potassium sheet, the diaphragm is made of glass fiber, and the electrolyte is 5 mol of KFSI in DIGLYME solution.
The assembled potassium ion battery was subjected to battery performance tests, the test results being 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 is as follows: weighing 0.003 mol of Bi (NO) according to the molecular formula3)3·5H2O and 0.003 mol FeCl3Adding into an agate ball milling tank. Then 2 mL of diluted 10% aqueous hydrochloric acid, 3mL of water, and 3mL of absolute ethanol were added in this order. Setting the ball milling speed at 700 rpm-1The ball milling time is 5 h;
the second step: collecting ball-milled products in a centrifuge tube, and setting the centrifuge speed to 10000 r min-1And the centrifugation time is 10min, deionized water is used for washing for 3 times, the washed product is collected in the centrifugation process, the water solution and unreacted substances are removed, and drying and grinding are carried out.
Example 4:
a preparation method of BiOCl and a multiphase composite semiconductor material thereof comprises the following steps:
the first step is as follows: weighing 0.002 mol of Bi (NO) according to the molecular formula3)3·5H2O and 0.004mol of CoCl2·6H2And adding O into an agate ball milling tank. Then 2 mL of diluted 10% aqueous hydrochloric acid, 3mL of water, and 3mL of absolute ethanol were added in this order. Setting the ball milling speed at 500 rpm-1The ball milling time is 5 h;
the second step is that: collecting ball-milled products in a centrifuge tube, and setting the centrifuge speed to 10000 r min-1And the centrifugation time is 10min, deionized water is used for washing for 3 times, the washed product is collected in the centrifugation process, the water solution and unreacted substances are removed, and drying and grinding are carried out.
Example 5:
a preparation method of BiOCl and a multiphase composite semiconductor material thereof comprises the following steps:
the first step is as follows: weighing 0.004mol of Bi (NO) according to the molecular formula3)3·5H2O and 0.002 mol of NiCl2·6H2And adding O into an agate ball milling tank. Then 2 mL of diluted 10% aqueous hydrochloric acid, 3mL of water, and 3mL of absolute ethanol were added in this order. Setting the ball milling rotating speed at 600 r min-1The ball milling time is 3 h;
the second step is that: collecting ball-milled products in a centrifuge tube, and setting the centrifugal speed to 9000 r min-1And the centrifugation time is 10min, deionized water is used for washing for 3 times, the washed product is collected in the centrifugation process, the water solution and unreacted substances are removed, and drying and grinding are carried out.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. A preparation method of BiOCl and a multiphase composite semiconductor material thereof is characterized in that: the raw materials of the BiOCl and the multiphase composite semiconductor material thereof are 0.002-0.006 mol of bismuth nitrate, 2 mL of diluted 10% hydrochloric acid aqueous solution, 3mL of ultrapure water, 3mL of anhydrous ethanol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony, and a single-phase BiOCl material or a BiOCl-based multiphase composite semiconductor material is obtained through physical ball milling and a centrifugal process.
2. The method for preparing BiOCl and the multiphase composite semiconductor material thereof according to claim 1, which comprises the following steps:
the first step is as follows: uniformly mixing 0.002-0.006 mol of bismuth nitrate, 2 mL of diluted 10% hydrochloric acid aqueous solution, 3mL of ultrapure water, 3mL of anhydrous ethanol and 0-0.004mol of metal chloride of cobalt, iron, aluminum, titanium, nickel, indium, manganese, copper, magnesium or antimony element by using a physical ball milling method to obtain a ball-milled product;
the second step is that: and removing unreacted impurities in the obtained ball-milling product through a centrifugal process to obtain the single-phase BiOCl material or the BiOCl-based multiphase composite material.
3. The method for preparing BiOCl and the multiphase composite semiconductor material thereof according to claim 2, wherein the method comprises the following steps: the physical ball milling method in the first step is that the ball milling rotating speed is 400--1And the ball milling time is 0.5-6 h.
4. The method for preparing BiOCl and the multiphase composite semiconductor material thereof according to claim 2, wherein the method comprises the following steps: the centrifugation step in the second step is that the centrifugation rotating speed is 5000-10000 r min-1Centrifuging for 10min, washing with deionized water for 3 times, collecting washed product, removing water solution and unreacted material, oven drying, and grinding.
5. The use of BiOCl and its multiphase composite semiconductor material as defined in claim 1 in the photocatalytic degradation of organic pollutants.
6. The use of the BiOCl and the multiphase composite semiconductor material thereof in the negative electrode material of the potassium ion battery according to claim 1.
7. The use of BiOCl and its multiphase composite semiconductor material in the photocatalytic degradation of organic pollutants as claimed in claim 5, wherein: carrying out photocatalytic degradation on rhodamine B (RhB) under a 300W xenon lamp light source, weighing 0.05 g of prepared single-phase BiOCl material or multi-phase composite semiconductor material thereof, adding the single-phase BiOCl material or the multi-phase composite semiconductor material thereof into a beaker containing 150 mL of 10 ppm RhB organic dye solution, putting the beaker into an ultrasonic cleaning machine, carrying out ultrasonic treatment for 5 min to carry out uniform dispersion, placing the beaker on a magnetic stirrer, and ensuring that the rotating speed can be kept at 600 rpm in the reaction process so that the prepared single-phase BiOCl material or the multi-phase composite semiconductor material thereof is continuously and uniformly dispersed in the organic solution in the degradation process; before a photocatalytic degradation experiment is carried out, a prepared solution of the single-phase BiOCl material or the multi-phase composite semiconductor material thereof needs to be placed in a dark condition for 30min in a dark room for adsorption, so that the prepared single-phase BiOCl material or the multi-phase composite semiconductor material thereof and RhB reach adsorption-desorption balance; then turning on a light source to carry out an illumination experiment, sampling a simulated organic pollutant aqueous solution every 5-10 min according to the photocatalytic degradation rate of different materials, taking 4 mL of reaction solution each time, and filtering out the photocatalyst by using an injection filter with the pore diameter of 0.22 mu m; the absorbance of the filtrate was analyzed using an ultraviolet-visible spectrophotometer at a RhB maximum absorption wavelength of 554 nm, and converted to the corresponding concentration with reference to a RhB standard curve.
8. The use of BiOCl and its multiphase composite semiconductor material in the negative electrode material of potassium ion battery as claimed in claim 6, wherein: in the assembly process of the potassium ion battery, the BiOCl material or the 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-methyl pyrrolidone) for 6 hours; uniformly coating the mixture on a copper foil by using a scraper through a tape casting method; and (3) carrying out button cell assembly operation in an argon atmosphere glove box, wherein the counter electrode is a potassium sheet, the diaphragm is made of glass fiber, and the electrolyte is 5 mol of KFSI in DIGLYME solution.
9. The use of BiOCl and its multiphase composite semiconductor material in the negative electrode material of potassium ion battery according to claim 8, characterized in that: the BiOCl material or the multiphase composite semiconductor material thereof, the acetylene black and the PVDF material correspond to 0.5 mL of NMP per 100 mg.
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