CN109201100A - A kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7Nanocomposite and preparation method thereof - Google Patents
A kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7Nanocomposite and preparation method thereof Download PDFInfo
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- CN109201100A CN109201100A CN201810840791.7A CN201810840791A CN109201100A CN 109201100 A CN109201100 A CN 109201100A CN 201810840791 A CN201810840791 A CN 201810840791A CN 109201100 A CN109201100 A CN 109201100A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 63
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052709 silver Inorganic materials 0.000 claims abstract description 55
- 239000002114 nanocomposite Substances 0.000 claims abstract description 54
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 230000008021 deposition Effects 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 239000002994 raw material Substances 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 9
- 239000001509 sodium citrate Substances 0.000 claims description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 5
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 229940045105 silver iodide Drugs 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 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 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000000527 sonication Methods 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- 239000011449 brick Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229910001430 chromium ion Inorganic materials 0.000 abstract description 2
- 238000007540 photo-reduction reaction Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 101710134784 Agnoprotein Proteins 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- 210000003127 knee Anatomy 0.000 description 2
- 238000004768 lowest unoccupied molecular orbital Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 231100000749 chronicity Toxicity 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- FDPIMTJIUBPUKL-UHFFFAOYSA-N dimethylacetone Natural products CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910006362 δ-Bi2O3 Inorganic materials 0.000 description 1
Classifications
-
- 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
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7Nanocomposite and preparation method thereof, the nanocomposite are g-C3N4、Bi4O7, silver nano-grain composition trielement composite material, wherein g-C3N4With laminar structured, silver nano-grain is dispersed in g-C3N4Lamella on, g-C3N4With Bi4O7It is built into Z-type heterojunction structure, and there is sharp interface；In the nanocomposite, the content of silver nano-grain is 1~10wt%, Bi4O7Content be 10~80wt%, silver nano-grain and Bi4O7Crystallization is good.A kind of Z-type hetero-junctions g-C of load silver is prepared using the method that repeatedly heat treatment combines light deposition in the present invention3N4@Bi4O7Nanocomposite.The nanocomposite each component content is adjustable, and adjustable extent is big, it is seen that photo-reduction metal chromium ions efficiency is good.
Description
Technical field
The present invention relates to Material Fields, more particularly, to a kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7It is nano combined
Material and preparation method thereof.
Background technique
With the rapid development of industry, Heavy Metals in Water Environment ionic soil is got worse, and common heavy metal ion is dirty
Dye is primarily referred to as mercury, lead, chromium, uranium etc..Since heavy metal ion toxicity is big, is difficult to degrade, and there is chronicity and accumulation property, holds
It is easily enriched in vivo, and then humans and animals vivo protein and enzyme denaturation is caused to inactivate, seriously threaten biology and the mankind's
Health.The common method of processing Heavy Metals in Waters has the precipitation method, extraction, absorption method and membrane separation process etc. at present, these sides
Fado can be along with energy consumption is high, processing is not thorough, secondary pollution problems.It is using photochemical catalyst redox heavy metal ion
A kind of novel heavy metal ion processing technique developed in recent years, can be synchronous to remove in environment under normal temperature and pressure conditions
Oxidized and reduced pollutant, reaction thoroughly and do not generate secondary pollution, shows in processing effluent containing heavy metal ions
Unique advantage, the concern by more and more people.
1989, the researcher in California, USA university Berli gram branch school synthesized successfully beta-phase carbon nitride (β-for the first time
C3N4), so that carbonitride (C3N4) initially enter the visual field of scientific research academia.1996, Virginia, US Polytechnics
Researcher is calculated by first principle demonstration and has deduced carbonitride and have 5 kinds of structures, be respectively α phase, β phase, quasi- cubic phase,
Cubic phase and class graphite-phase (g-C3N4).2009, Wang etc. reported g-C on Nature Materials for the first time3N4In light
Application in catalysis.g-C3N4Highest occupied molecular orbital (HOMO ,+1.4V) and lowest unoccupied molecular orbital (LUMO ,-
Band gap between 1.3V) is 2.7eV, therefore has certain visible light-responded ability.
Bismuth-based oxide is a kind of novel catalysis material, and common Bi-O system is containing there are many phases, such as Bi2O3(point
For four kinds of crystal form α-, β-, γ-and δ-Bi2O3), Bi2O4, Bi2O2-x, Bi8O11, Bi6O7, Bi4O7And BiO.Hu etc. is reported not
When synthermal lower sintering, Bi2O4Significant transformation behavior is shown, and is prepared for a series of bismuth oxide material (Bi4O7, α-
Bi2O3With β-Bi2O3), it the article pointed out Bi2O4It can be converted Bi at 250 DEG C4O7。Bi4O7It is a kind of bismuthino of mixed valence
Oxide, bandwidth 1.89eV, light absorption cutoff wavelength belong to narrow bandgap semiconductor material at 656nm, and having can
Light-exposed absorbability.
In the research of photocatalysis at present it is the most commonly used it is two kinds of it is heterogeneous become II type hetero-junctions and Z-type hetero-junctions, II
Type hetero-junctions is different the carrier transfer path in separation process with Z-type hetero-junctions photo-generate electron-hole.For II type
Hetero-junctions, the conduction band and valence band location of two kinds of semiconductors are close, and band curvature, light can be generated at contact interface after the two contact
Raw electrons are shifted along interface knee, and equally, photohole can also be shifted along interface knee, just realize partly lead in this way
The separation of the photo-generate electron-hole pair of body-semiconductor composite under light illumination.For Z-type hetero-junctions, carrier transfer
Path and II type hetero-junctions are entirely different, when the valence band of one of semiconductor connects compared with the conduction band positions of another semiconductor
When close, light induced electron meeting and photohole can be compound inside two kinds of semiconductor contact interfaces, and in turn, two kinds of semiconductors generate
Light induced electron and photohole can remain respectively, carry out subsequent photo catalytic reduction/oxidation reaction.
2008, Japanese AWAZU etc. had developed the Ag/TiO for having wide spectrum Absorption Characteristics in visible light region2Light is urged
Change material, the surface plasma body resonant vibrations of the discovery noble metal nano particles such as Au, Ag (Surface Plasmon Resonance,
SPR) there is apparent improvement result to the photocatalytic activity of semiconductor, and be prepared for a variety of Ag (Au)/partly lead on this basis
Body nano composite photo-catalyst has been put forward for the first time surface plasma photochemical catalyst (Plasmonic Photocatalyst)
Concept.Since then, SPR has received the concern of more and more researchers to the research of the visible light photocatalysis active of optimization semiconductor.
Chinese patent CN107398293A discloses a kind of Z-type photochemical catalyst TiO2/g-C3N4Preparation method, by quiet
Electrospun and in-situ crystallization calcination method, method of electrostatic spinning operation is difficult to control, and TiO2For wide bandgap semiconductor materials, although structure
Z-type structure is built, but visible light activity improvement is still limited.Chinese patent CN106975507A discloses a kind of Ag/g-C3N4It is multiple
The preparation method of light combination catalyst, this method are g-C with melamine3N4Raw material, the g-C of preparation3N4Lamella fuzzy, than
Surface area is little.
Summary of the invention
To overcome the above-mentioned problems in the prior art, the object of the present invention is to provide a kind of Z-type of load silver is heterogeneous
Tie g-C3N4@Bi4O7Nanocomposite and preparation method thereof, the nanocomposite each component content is adjustable, and adjustable extent
Greatly, it is seen that photo-reduction metal chromium ions efficiency is good.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7Nanocomposite, the nanocomposite are g-C3N4、
Bi4O7, silver nano-grain composition trielement composite material, wherein g-C3N4With laminar structured, silver nano-grain uniformly divides
It is dispersed in g-C3N4Lamella on, g-C3N4With Bi4O7It is built into Z-type heterojunction structure, and there is sharp interface；It is described nano combined
In material, the content of silver nano-grain is 1~10wt%, Bi4O7Content be 10~80wt%.
The specific surface area of the nanocomposite is 60~100m2g-1, silver nano-grain partial size is 10~20nm.
A kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7The preparation method of nanocomposite, comprising the following steps:
(1) g-C will be prepared3N4Raw material carry out thermal polycondensation in air atmosphere, obtain block shape g-C3N4；
(2) the block shape g-C for taking step (1) to obtain3N4Hot soarfing is carried out in air atmosphere from obtaining g-C3N4Nanometer sheet；
(3) Bi will be prepared4O7Stock dispersion in deionized water, then carry out hydro-thermal process, obtained after dry brick-red
Powder；
(4) g-C that the brick-red powder and step (2) for taking step (3) to obtain obtain3N4Nanometer sheet is dispersed in organic solvent
In, ultrasonic treatment to uniform mixing；Then drying is volatilized completely to organic solvent, then obtained mixed-powder is transferred to Muffle
In furnace, calcining obtains Z-type hetero-junctions g-C in air atmosphere3N4@Bi4O7Nanocomposite；
(5) the Z-type hetero-junctions g-C for obtaining step (4)3N4@Bi4O7Nanocomposite disperses in deionized water, to surpass
Sonication is to evenly dispersed；Addition prepares the raw material and hole sacrifice agent of silver nano-grain, obtains the Z of load silver by light deposition
Type hetero-junctions g-C3N4@Bi4O7Nanocomposite.
In step (1), g-C is prepared3N4Raw material be one of urea, melamine, dicyandiamide or cyanamide or a variety of
Mixture；The condition of thermal polycondensation are as follows: temperature is 400~700 DEG C, and the time is 2~5 hours, and heating rate is 1~5 DEG C/min.
In step (2), hot soarfing from condition are as follows: temperature be 450~750 DEG C, the time be 3~6 hours, heating rate 1
~10 DEG C/min.
In step (3), Bi is prepared4O7Raw material be sodium bismuthate, bismuth nitrate one or more mixtures；Prepare Bi4O7
Raw material in deionized water concentration be 5~20mg/mL；The condition of hydro-thermal process are as follows: temperature is 120~200 DEG C, the time 4
~12 hours.
In step (4), organic solvent is ethyl alcohol, methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, tetrahydrofuran, diformazan
One kind of ether or acetone；Brick-red powder and g-C3N4The mass ratio of nanometer sheet is 0.1~0.8, and two kinds of powder are in organic solvent
Total concentration be 2~10mg/mL.
In step (4), the condition of calcining are as follows: temperature is 200~350 DEG C, and the time is 2~5 hours, and heating rate is 1~5
℃/min。
In step (5), prepares the raw material of silver nano-grain and mixed for silver nitrate, silver chlorate, the one or more of silver iodide
Close object；Hole sacrifice agent is one or more mixtures of sodium citrate, methanol, ethylene glycol；Z-type hetero-junctions g-C3N4@
Bi4O7Concentration is 0.1~2mg/mL to nanocomposite in deionized water；The raw material of silver nano-grain is prepared in deionized water
Middle concentration is 0.5~2mM；Concentration is 0.5~2mM to hole sacrifice agent in deionized water；Prepare the raw material of silver nano-grain with
The molar ratio of hole sacrifice agent is 1:1~1:2.
In step (5), the condition of light deposition are as follows: 200~700nm of wavelength, 40~70W of power, luminous range be 20~
40cm, light application time are 0.5~3 hour.
The utility model has the advantages that the present invention is respectively with urea, melamine, dicyandiamide g-C3N4Raw material, with sodium bismuthate, nitric acid
Bismuth is Bi4O7Raw material light deposition is combined using multiple heat treatment using silver nitrate, silver chlorate, silver iodide as the raw material of nano silver
Method, be prepared for it is a kind of load silver Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.The composite material has larger
Specific surface area, Z-type heterojunction boundary is obvious, and silver nano-grain is uniform, your gold of Z-type hetero-junctions-can be cooperateed in photocatalytic process
The effect of metal surface plasma resonance.
Compared with prior art, the present invention has obtained a kind of load silver using the method that repeatedly heat treatment combines light deposition
Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.By controlling heat treatment process, different g-C are prepared3N4Pattern；Pass through
Deploy Bi4O7And g-C3N4Feed ratio, construct Z-type heterojunction structure, and deploy Bi4O7And g-C3N4Mass ratio.Pass through control
Light deposition process controls the size and content of Ag nano particle.
The Z-type hetero-junctions g-C of load silver prepared by the present invention3N4@Bi4O7Nanocomposite has biggish specific surface
Product (60~100m2g-1), Z-type heterojunction boundary is obvious, and silver nano-grain is dispersed in g-C3N4Lamella on, silver nanoparticle
Grain partial size is in 10~20nm.In trielement composite material, silver content is 1~10wt%, Bi4O7Content is about 10~80wt%.This is multiple
Condensation material has good absorbing properties, especially in visible-range, compared with block shape g-C3N4And g-C3N4Nanometer sheet is inhaled
Receipts are remarkably reinforced.g-C3N4With Bi4O7The Z-type heterojunction structure of building promotes the separation of electron hole, with SPR performance
Nano silver further promotes the reducing property of light induced electron.Pass through (420~700nm of wavelength), heavy metal chromium under visible light conditions
The analysis of ion (Cr (VI)) reducing property, the degradation efficiency of the trielement composite material is approximately block shape g-C3N430~50 times,
Heavy metal ion in processing industrial wastewater has broad application prospects.
Detailed description of the invention
Fig. 1 is block shape g-C prepared by embodiment 13N4(Bulk g-C3N4) and g-C3N4Nanometer sheet characteristic X-ray spreads out
Penetrate (XRD) map；
Fig. 2 is g-C prepared by embodiment 23N4@Bi4O7With Ag@g-C3N4@Bi4O7Composite material distinctive X-ray diffraction
(XRD) map；
Fig. 3 is block shape g-C prepared by embodiment 1 and embodiment 23N4、g-C3N4Nanometer sheet, g-C3N4@Bi4O7With Ag@
g-C3N4@Bi4O7Composite material feature nitrogen adsorption-desorption isotherm (BET)；
Fig. 4 is g-C prepared by embodiment 23N4@Bi4O7With Ag@g-C3N4@Bi4O7The transmission electron microscopy of composite material
Mirror (TEM) figure and high power transmission electron microscope (HRTEM)；
Fig. 5 is g-C prepared by embodiment 1 and embodiment 33N4Nanometer sheet, g-C3N4@Bi4O7With Ag@g-C3N4@Bi4O7
Composite material fluorescence spectra (PL)；
Fig. 6 is g-C prepared by embodiment 1 and embodiment 43N4Nanometer sheet, g-C3N4@Bi4O7With Ag@g-C3N4@Bi4O7
Composite material ultraviolet-visible absorption spectroscopy；
Fig. 7 is Ag@g-C prepared by embodiment 53N4@Bi4O7Transmission electron microscope (TEM) figure of composite material；
Fig. 8 is Ag@g-C prepared by embodiment 63N4@Bi4O7Transmission electron microscope (TEM) figure of composite material.
Specific embodiment
A kind of Z-type hetero-junctions g-C of load silver of the invention3N4@Bi4O7Nanocomposite, the nanocomposite are
g-C3N4、Bi4O7, silver nano-grain composition trielement composite material, wherein g-C3N4With laminar structured, silver nano-grain
It is dispersed in g-C3N4Lamella on, g-C3N4With Bi4O7It is built into Z-type heterojunction structure, and there is sharp interface；It is described to receive
In nano composite material, the content of silver nano-grain is 1~10wt%, Bi4O7Content be 10~80wt%, silver nano-grain and
Bi4O7Crystallization is good.
Wherein, the specific surface area of nanocomposite is 60~100m2g-1, silver nano-grain partial size is 10~20nm.
A kind of Z-type hetero-junctions g-C of load silver of the invention3N4@Bi4O7The preparation method of nanocomposite, including with
Lower step:
(1) g-C will be prepared3N4Raw material carry out thermal polycondensation in air atmosphere, obtain block shape g-C3N4；
Wherein, g-C is prepared3N4Raw material be one of urea, melamine, dicyandiamide or cyanamide or a variety of mixed
Close object；The condition of thermal polycondensation are as follows: temperature is 400~700 DEG C, and the time is 2~5 hours, and heating rate is 1~5 DEG C/min；
(2) the block shape g-C for taking step (1) to obtain3N4Hot soarfing is carried out in air atmosphere from obtaining g-C3N4Nanometer sheet；
Wherein, hot soarfing from condition are as follows: temperature be 450~750 DEG C, the time be 3~6 hours, heating rate be 1~10
℃/min；
(3) Bi will be prepared4O7Stock dispersion in deionized water, then carry out hydro-thermal process, obtained after dry brick-red
Powder；
Wherein, Bi is prepared4O7Raw material be sodium bismuthate, bismuth nitrate one or more mixtures；Prepare Bi4O7Original
Concentration is 5~20mg/mL to material in deionized water；The condition of hydro-thermal process are as follows: temperature is 120~200 DEG C, and the time is 4~12
Hour；
(4) g-C that the brick-red powder and step (2) for taking step (3) to obtain obtain3N4Nanometer sheet is dispersed in organic solvent
In, ultrasonic treatment to uniform mixing；Then drying is volatilized completely to organic solvent, then obtained mixed-powder is transferred to Muffle
In furnace, calcining obtains Z-type hetero-junctions g-C in air atmosphere3N4@Bi4O7Nanocomposite；
Wherein, organic solvent be ethyl alcohol, methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, tetrahydrofuran, dimethyl ether or
One kind of acetone；Brick-red powder and g-C3N4The mass ratio of nanometer sheet is 0.1~0.8, two kinds of powder in organic solvent total
Concentration is 2~10mg/mL；The condition of calcining are as follows: temperature is 200~350 DEG C, and the time is 2~5 hours, and heating rate is 1~5
℃/min；
(5) the Z-type hetero-junctions g-C for obtaining step (4)3N4@Bi4O7Nanocomposite disperses in deionized water, to surpass
Sonication is to evenly dispersed；Addition prepares the raw material and hole sacrifice agent of silver nano-grain, obtains the Z of load silver by light deposition
Type hetero-junctions g-C3N4@Bi4O7Nanocomposite；
Wherein, the raw material for preparing silver nano-grain is one or more mixtures of silver nitrate, silver chlorate, silver iodide；
Hole sacrifice agent is one or more mixtures of sodium citrate, methanol, ethylene glycol；Z-type hetero-junctions g-C3N4@Bi4O7Nanometer
Concentration is 0.1~2mg/mL to composite material in deionized water；Preparing the raw material of silver nano-grain, concentration is in deionized water
0.5~2mM；Concentration is 0.5~2mM to hole sacrifice agent in deionized water；Prepare the raw material and hole sacrifice of silver nano-grain
The molar ratio of agent is 1:1~1:2；The condition of light deposition are as follows: 200~700nm of wavelength, 40~70W of power, luminous range be 20~
40cm, light application time are 0.5~3 hour.
The present invention is described in detail combined with specific embodiments below.
Protection scope of the present invention is not limited to embodiment, and only protection is specifically addressed.For example, graphite-phase in embodiment
The raw material of carbonitride selects dicyandiamide, can also select urea, melamine or cyanamide replacement；Hole is sacrificial during light deposition
What domestic animal agent was selected is sodium citrate, is also possible to methanol, ethylene glycol replacement.The raw material of nano silver is silver nitrate, is also possible to chlorine
Change silver, silver iodide, the organic solvent of dispersed sample can also use methanol, ethyl alcohol, normal propyl alcohol, isopropanol, just in addition to ethyl alcohol
Butanol, tetrahydrofuran, dimethyl ether or acetone.
Embodiment 1
Weigh 10g dicyandiamide addition have in the alumina crucible of lid, under the conditions of air atmosphere, Muffle furnace with 2 DEG C/
Min heating rate is warming up to 550 DEG C, keeps the temperature 4 hours, and obtaining yellow powder sample is block shape g-C3N4.By block shape g-C3N4
It is laid in uncovered ceramics Noah's ark bottom.Under the conditions of air atmosphere, Muffle furnace is warming up to 500 DEG C with the heating rate of 5 DEG C/min,
It is kept for 3 hours, obtained pale yellow powder sample, as g-C3N4Nanometer sheet.
Embodiment 2
By 0.7g sodium bismuthate (NaBiO3) be distributed in 75mL water, it is transferred to 100mL polytetrafluoroethyllining lining later not
It becomes rusty in steel water heating kettle, is then heated 6 hours at 160 DEG C using baking oven.After reaction, red-brown precipitation object passes through centrifuge separation,
It is dried after deionized water washing, obtained brick-red powder.It takes 60mL ethyl alcohol, the brick-red powder of 0.084g and 0.21g is added
g-C3N4Nanometer sheet is ultrasonically treated 50min.By dispersion liquid at 60 DEG C the dry removing of volatilization in 4 hours ethyl alcohol, then will obtain
Powder is put into crucible with cover, is warming up at 250 DEG C and is heated 3 hours with the heating rate of 2 DEG C/min in Muffle furnace, obtained
Sample is Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite is abbreviated as g-C3N4@Bi4O7。
By 500mg Bi4O7@g-C3N4Composite material is dispersed in 500mL deionized water, then ultrasound 60min.It is mixed to this
It closes and 0.8g AgNO is added in solution3With 0.15g sodium citrate.After stirring 40min, suspension is transferred to the UV lamp case of sealing
It is middle to irradiate 60min with UV light (wavelength 365nm, power 56W, operating distance 30cm).Finally, deionized water centrifuge washing, dry
Obtaining sample afterwards is the Z-type hetero-junctions g-C for loading silver3N4@Bi4O7Nanocomposite is abbreviated as Ag@g-C3N4@Bi4O7。
Embodiment 3
By 0.7g sodium bismuthate (NaBiO3) be distributed in 100mL water, it is transferred to 100mL polytetrafluoroethyllining lining later not
It becomes rusty in steel water heating kettle, is then heated 6 hours at 200 DEG C using baking oven.After reaction, red-brown precipitation object passes through centrifuge separation,
It is dried after deionized water washing, obtained brick-red powder.It takes 60mL ethyl alcohol, the brick-red powder of 0.021g and 0.21g is added
g-C3N4Nanometer sheet (g-C3N4The preparation of nanometer sheet is with embodiment 1), it is ultrasonically treated 50min.By dispersion liquid dry 4 at 60 DEG C
Hour volatilization removes ethyl alcohol, is then put into obtained powder in crucible with cover, with the heating speed of 2 DEG C/min in Muffle furnace
Rate is warming up at 300 DEG C and heats 3 hours, and obtaining sample is Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.
By 500mg Bi4O7@g-C3N4Composite material is dispersed in 500mL deionized water, then ultrasound 60min.It is mixed to this
It closes and 0.8g AgNO is added in solution3With 0.15g sodium citrate.After stirring 40min, suspension is transferred to the UV lamp case of sealing
It is middle to irradiate 60min with UV light (wavelength 365nm, power 56W, operating distance 30cm).Finally, deionized water centrifuge washing, dry
Obtaining sample afterwards is the Z-type hetero-junctions g-C for loading silver3N4@Bi4O7Nanocomposite.
Embodiment 4
By 0.7g sodium bismuthate (NaBiO3) be distributed in 50mL water, it is transferred to 100mL polytetrafluoroethyllining lining later not
It becomes rusty in steel water heating kettle, is then heated 6 hours at 160 DEG C using baking oven.After reaction, red-brown precipitation object passes through centrifuge separation,
It is dried after deionized water washing, obtained brick-red powder.It takes 60mL ethyl alcohol, the brick-red powder of 0.042g and 0.21g is added
g-C3N4Nanometer sheet (g-C3N4The preparation of nanometer sheet is with embodiment 1), it is ultrasonically treated 50min.By dispersion liquid dry 4 at 60 DEG C
Hour volatilization removes ethyl alcohol, is then put into obtained powder in crucible with cover, with the heating speed of 2 DEG C/min in Muffle furnace
Rate is warming up at 250 DEG C and heats 3 hours, and must obtain sample is Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.
By 500mg Bi4O7@g-C3N4Composite material is dispersed in 500mL deionized water, then ultrasound 60min.It is mixed to this
It closes and 0.8g AgNO is added in solution3With 0.20g sodium citrate.After stirring 40min, suspension is transferred to the UV lamp case of sealing
It is middle to be irradiated 2 hours with UV light (wavelength 365nm, power 56W, operating distance 30cm).Finally, deionized water centrifuge washing, dry
Obtaining sample afterwards is the Z-type hetero-junctions g-C for loading silver3N4@Bi4O7Nanocomposite.
Embodiment 5
By 0.7g sodium bismuthate (NaBiO3) be distributed in 75mL water, it is transferred to 100mL polytetrafluoroethyllining lining later not
It becomes rusty in steel water heating kettle, is then heated 6 hours at 160 DEG C using baking oven.After reaction, red-brown precipitation object passes through centrifuge separation,
It is dried after deionized water washing, obtained brick-red powder.It takes 60mL ethyl alcohol, the brick-red powder of 0.126g and 0.21g is added
g-C3N4Nanometer sheet (g-C3N4The preparation of nanometer sheet is with embodiment 1), it is ultrasonically treated 50min.By dispersion liquid dry 4 at 60 DEG C
Hour volatilization removes ethyl alcohol, is then put into obtained powder in crucible with cover, with the heating speed of 2 DEG C/min in Muffle furnace
Rate is warming up at 250 DEG C and heats 3 hours, and obtaining sample is Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.
By 500mg Bi4O7@g-C3N4Composite material is dispersed in 500mL deionized water, then ultrasound 60min.It is mixed to this
It closes and 0.8g AgNO is added in solution3With 0.15g sodium citrate.After stirring 40min, suspension is transferred to the UV lamp case of sealing
It is middle to be irradiated 1.5 hours with UV light (wavelength 365nm, power 56W, operating distance 30cm).Finally, deionized water centrifuge washing, does
It is the Z-type hetero-junctions g-C for loading silver that sample is obtained after dry3N4@Bi4O7Nanocomposite.
Embodiment 6
By 0.7g sodium bismuthate (NaBiO3) be distributed in 50mL water, it is transferred to 100mL polytetrafluoroethyllining lining later not
It becomes rusty in steel water heating kettle, is then heated 6 hours at 160 DEG C using baking oven.After reaction, red-brown precipitation object passes through centrifuge separation,
It is dried after deionized water washing, obtained brick-red powder.It takes 60mL ethyl alcohol, the brick-red powder of 0.168g and 0.21g is added
g-C3N4Nanometer sheet is ultrasonically treated 50min.By dispersion liquid at 60 DEG C the dry removing of volatilization in 4 hours ethyl alcohol, then will obtain
Powder is put into crucible with cover, is warming up at 250 DEG C and is heated 3 hours with the heating rate of 2 DEG C/min in Muffle furnace, obtained
Sample is Z-type hetero-junctions g-C3N4@Bi4O7Nanocomposite.
By 500mg Bi4O7@g-C3N4Composite material is dispersed in 500mL deionized water, then ultrasound 60min.It is mixed to this
It closes and 0.8g AgNO is added in solution3With 0.15g sodium citrate.After stirring 40min, suspension is transferred to the UV lamp case of sealing
It is middle to irradiate 60min with UV light (wavelength 365nm, power 56W, operating distance 30cm).Finally, deionized water centrifuge washing, dry
Obtaining sample afterwards is the Z-type hetero-junctions g-C for loading silver3N4@Bi4O7Nanocomposite.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of Z-type hetero-junctions g-C of load silver3N4@Bi4O7Nanocomposite, it is characterised in that: the nanocomposite is
g-C3N4、Bi4O7, silver nano-grain composition trielement composite material, wherein g-C3N4With laminar structured, silver nano-grain
It is dispersed in g-C3N4Lamella on, g-C3N4With Bi4O7It is built into Z-type heterojunction structure, and there is sharp interface；It is described to receive
In nano composite material, the content of silver nano-grain is 1~10wt%, Bi4O7Content be 10~80wt%.
2. the Z-type hetero-junctions g-C of load silver according to claim 13N4@Bi4O7Nanocomposite, it is characterised in that:
The specific surface area of the nanocomposite is 60~100m2g-1, silver nano-grain partial size is 10~20nm.
3. a kind of Z-type hetero-junctions g-C of any load silver of claims 1 or 23N4@Bi4O7The preparation of nanocomposite
Method, it is characterised in that: the following steps are included:
(1) g-C will be prepared3N4Raw material carry out thermal polycondensation in air atmosphere, obtain block shape g-C3N4；
(2) the block shape g-C for taking step (1) to obtain3N4Hot soarfing is carried out in air atmosphere from obtaining g-C3N4Nanometer sheet；
(3) Bi will be prepared4O7Stock dispersion in deionized water, then carry out hydro-thermal process, obtain brick red toner after dry
End；
(4) g-C that the brick-red powder and step (2) for taking step (3) to obtain obtain3N4Nanometer sheet disperses in organic solvent, to surpass
Sonication is mixed to uniform；Then drying is volatilized completely to organic solvent, then obtained mixed-powder is transferred in Muffle furnace,
Calcining obtains Z-type hetero-junctions g-C in air atmosphere3N4@Bi4O7Nanocomposite；
(5) the Z-type hetero-junctions g-C for obtaining step (4)3N4@Bi4O7Nanocomposite disperses in deionized water, at ultrasound
It manages to evenly dispersed；Addition prepares the raw material and hole sacrifice agent of silver nano-grain, and the Z-type for obtaining load silver by light deposition is different
Matter knot g-C3N4@Bi4O7Nanocomposite.
4. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
It is characterized in that: in step (1), preparing g-C3N4Raw material be one of urea, melamine, dicyandiamide or cyanamide or more
The mixture of kind；The condition of thermal polycondensation are as follows: temperature be 400~700 DEG C, the time be 2~5 hours, heating rate be 1~5 DEG C/
min。
5. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
Be characterized in that: in step (2), hot soarfing from condition are as follows: temperature be 450~750 DEG C, the time be 3~6 hours, heating rate 1
~10 DEG C/min.
6. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
It is characterized in that: in step (3), preparing Bi4O7Raw material be sodium bismuthate, bismuth nitrate one or more mixtures；Preparation
Bi4O7Raw material in deionized water concentration be 5~20mg/mL；The condition of hydro-thermal process are as follows: temperature is 120~200 DEG C, the time
It is 4~12 hours.
7. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
Be characterized in that: in step (4), organic solvent is ethyl alcohol, methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, tetrahydrofuran, two
One kind of methyl ether or acetone；Brick-red powder and g-C3N4The mass ratio of nanometer sheet is 0.1~0.8, and two kinds of powder are in organic solvent
In total concentration be 2~10mg/mL.
8. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
Be characterized in that: in step (4), the condition of calcining are as follows: temperature be 200~350 DEG C, the time be 2~5 hours, heating rate be 1~
5℃/min。
9. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
It is characterized in that: in step (5), preparing the raw material of silver nano-grain and mixed for silver nitrate, silver chlorate, the one or more of silver iodide
Close object；Hole sacrifice agent is one or more mixtures of sodium citrate, methanol, ethylene glycol；Z-type hetero-junctions g-C3N4@
Bi4O7Concentration is 0.1~2mg/mL to nanocomposite in deionized water；The raw material of silver nano-grain is prepared in deionized water
Middle concentration is 0.5~2mM；Concentration is 0.5~2mM to hole sacrifice agent in deionized water；Prepare the raw material of silver nano-grain with
The molar ratio of hole sacrifice agent is 1:1~1:2.
10. the Z-type hetero-junctions g-C of load silver according to claim 33N4@Bi4O7The preparation method of nanocomposite,
It is characterized by: in step (5), the condition of light deposition are as follows: 200~700nm of wavelength, 40~70W of power, luminous range is 20~
40cm, light application time are 0.5~3 hour.
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