CN108993572A - A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film - Google Patents
A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film Download PDFInfo
- Publication number
- CN108993572A CN108993572A CN201810900409.7A CN201810900409A CN108993572A CN 108993572 A CN108993572 A CN 108993572A CN 201810900409 A CN201810900409 A CN 201810900409A CN 108993572 A CN108993572 A CN 108993572A
- Authority
- CN
- China
- Prior art keywords
- film
- tungstic acid
- carbon compound
- fe2o3 doping
- nitridation carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 150000001722 carbon compounds Chemical class 0.000 title claims abstract description 30
- 238000001354 calcination Methods 0.000 claims abstract description 22
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004202 carbamide Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 2
- 229910052721 tungsten Inorganic materials 0.000 claims 2
- 239000010937 tungsten Substances 0.000 claims 2
- 239000010408 film Substances 0.000 abstract description 47
- 238000000034 method Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 8
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 3
- 230000008030 elimination Effects 0.000 abstract description 2
- 238000003379 elimination reaction Methods 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract 1
- 239000003403 water pollutant Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 238000001069 Raman spectroscopy Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010531 catalytic reduction reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009643 growth defect Effects 0.000 description 1
- -1 have sol-gel method Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000004304 visual acuity Effects 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
-
- B01J35/39—
-
- B01J35/59—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
Abstract
The present invention relates to a kind of preparation methods of Fe2O3 doping tungstic acid-nitridation carbon compound film, belong to technical field of material.The method of the present invention is that Fe2O3 doping WO is made using sodium tungstate and urea as raw material with hydro-thermal method in doping reagent with ferric nitrate3Thin-film material, by being impregnated in urea liquid, dry, calcining and etc. after, prepare Fe2O3 doping tungstic acid-nitridation carbon compound film, there is good elimination performance to heavy metal contaminants in water.This method has the advantages that equipment and simple process, preparation cost are low etc..Film surface obtained is smooth, and particle size distribution is uniform, and thin film stability is good；This material has good application prospect in terms of photocatalysis water pollutant.
Description
Technical field
The present invention relates to a kind of preparation methods of Fe2O3 doping tungstic acid-nitridation carbon compound film, belong to material preparation skill
Art field.
Background technique
WO3Semiconductor light-catalyst is considered as one of ideal photocatalyst material, it has a characteristic that green nothing
Poison, preparation is simple, physicochemical properties are stable, sensitive to visible light, electronic transmission performance is good, raw material are cheap.In gas
Detection, photocatalysis, the fields such as light shutter device and electrochromic device have a wide range of applications.But WO3Middle light induced electron-sky
The Quick Casting in cave pair constrains its photocatalysis efficiency to a certain extent.Therefore, effectively inhibit WO3Middle photo-generate electron-hole
Pair it is compound be to further increase WO3The effective way of photochemical catalyst efficiency.
Currently, for improving WO3The effective way of photocatalysis film device efficiency is concentrated mainly on and improves its electron hole
Separative efficiency, in terms of promoting its electron transfer efficiency.The method mainly used has metal ion mixing, semiconductor material compound
Deng.
Such as A.Hoel in 2004 is prepared for the WO of doping Al with high-frequency induction evaporation source vapour deposition method3Al is mixed in thick film, discovery
WO3Film is to H2The sensibility of S is than pure WO3Good, resolving power is pure WO33 times of film.Wang Xuan in 2010 etc. is with wolframic acid and the tetrabutyl
Ammonium hydroxide is raw material, prepares C by sol-gal process and adulterates WO3-x, the results showed that C doping changes WO to a certain extent3
Crystal structure, do not generate crystallography transformation under the premise of so that catalyst surface W5+Increase with Lacking oxygen content, these are arranged
It applies and all improves WO3-xAbsorbing properties and electronic transmission performance, to be conducive to the raising of photocatalytic activity.For another example 2012
Year Bi Dongqin etc. uses mechanical mix techniques, is prepared for WO3And Fe2O3Mixture, test result show be when calcination temperature
400 DEG C and Fe2O3Content mass percentage be 1.0% when, to the photocatalysis effect highest of organic dyestuff X3B.
Cui Yu people in 2011 etc. are prepared for complex phase photochemical catalyst WO3/ ZnO, and the processing to the waste water containing acid black dye
It is studied, finds complex phase photochemical catalyst WO3/ ZnO is obvious to the percent of decolourization effect of acid black dye solution, reachable
99.6%.White stamen in 2011 etc. is prepared for WO using sol-gel method3-TiO2Nanocomposite works as WO3Quality percentage contain
Amount is in 3%, when calcination temperature is 550 DEG C, the efficiency of photo-catalytic degradation of methyl-orange waste water from dyestuff, than pure WO3And TiO2Degradation effect
Rate is significantly improved.Faqi Zhan in 2015 is by WO3With g-C3N4It is compound, it was demonstrated that the composite material can promote light induced electron
With the separation in hole, to improve the catalytic efficiency of composite material.
WO at present3And its preparation method of laminated film mainly have sol-gel method, chemical meteorology deposition method, hydro-thermal and
Solvent-thermal method etc..The wherein low temperature of hydro-thermal method, high-pressure solution condition, are conducive to that growth defect is few, is orientated, the crystalline substance of perfect structure
Body, and that the product crystallinity synthesized is high, thermal stress is small, uniformity and purity are higher, granularity is easily-controllable and process costs are cheap etc. is excellent
Point.The present invention is that Fe2O3 doping WO is made using sodium tungstate and urea as raw material with hydro-thermal method in doping reagent with ferric nitrate3Film material
Expect (referring to the number of patent application 201810456659.6 of applicant), by impregnating, drying, calcining in urea liquid
And etc. after, prepare Fe2O3 doping tungstic acid-nitridation carbon compound film.The film has the pollutants such as heavy metal in water good
Good catalytic removal performance.
Summary of the invention
It is an object of the invention to propose a kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film；The party
Method is that Fe2O3 doping WO is made using sodium tungstate and urea as raw material with hydro-thermal method in doping reagent with ferric nitrate3Thin-film material passes through
Impregnated in urea liquid, be dry, calcining and etc. after, prepare Fe2O3 doping tungstic acid-nitridation carbon compound film.This is compound
Film has good catalytic removal performance to pollutants such as heavy metals in water.
Fe2O3 doping tungstic acid-nitridation carbon compound film preparation method, which is characterized in that the method passes through sodium tungstate
Hydrolysis, the doping of ferric nitrate and the calcining of composite urea are made, comprising the following steps:
(1) a certain amount of sodium tungstate and ferric nitrate are dissolved in distilled water, are stirred evenly；
(2) it is slowly added to a certain amount of hydrochloric acid solution in above-mentioned solution, be vigorously stirred；
(3) FTO electro-conductive glass is added in the above solution, carries out hydro-thermal reaction, then natural cooling；
(4) after the cleaning of above-mentioned FTO electro-conductive glass, drying, calcining, natural cooling；
(5) film sample obtained above is immersed into urea liquid, takes out dry, calcining, iron is made after natural cooling and mixes
Miscellaneous tungstic acid-nitridation carbon compound film.
In the above preparation method, the raw material in the step (1) is from tungstates and nitre such as sodium tungstate, ammonium tungstates
The molysite such as sour iron, iron chloride.
In the above preparation method, the step (1) and (2) middle operation carry out under stirring.
In the above preparation method, the temperature of hydro-thermal reaction is 80-200 DEG C in the step (3).
In the above preparation method, the soaking time in the step (3) under hydrothermal temperature is 12-48 hours.
In the above preparation method, cleaning is rinsed using deionized water in the step (4).
In the above preparation method, drying mode is dried in vacuo using 50-100 DEG C in the step (4).
In the above preparation method, the calcination temperature in the step (4) is 300-800 DEG C.
In the above preparation method, soaking time is 1-6 hours at calcination temperatures in the step (4).
In the above preparation method, the iron content of the middle gained WO 3 film of the step (4) is 0.3% to 5.0%
Between.
In the above preparation method, three oblique crystal phases and hexagonal phase in gained WO 3 film in the step (4)
Ratio is 1:4 between 3:5.
In the above preparation method, drying mode is dried in vacuo using 50-100 DEG C in the step (5).
In the above preparation method, the calcination temperature in the step (5) is 300-800 DEG C.
In the above preparation method, soaking time is 1-6 hours at calcination temperatures in the step (5).
In the above preparation method, carbonitride C in the middle gained laminated film of the step (5)3N4Mass percent be
Between 0.01% to 0.5%.
Fe2O3 doping tungstic acid-nitridation the carbon compound film prepared using this technology has equipment and simple process, preparation
The features such as condition is stringent controllable, low in cost, the film surface uniform ground of preparation, firmness is high, can Reusability, and light is urged
It is significant to change efficiency.
Detailed description of the invention
Fig. 1 is the tungstic acid of Fe2O3 doping prepared by the embodiment of the present invention 1-nitridation carbon compound film in photo catalytic reduction sexavalence
The pattern of the catalysis reaction front and back of chromium
Fig. 2 is the tungstic acid of Fe2O3 doping prepared by the embodiment of the present invention 1-nitridation carbon compound film stereoscan photograph
Fig. 3 be the tungstic acid of Fe2O3 doping prepared by the embodiment of the present invention 1-nitridation carbon compound film XRD spectrum (from upper and
Lower is C respectively3N4XRD test curve, Fe2O3 doping WO 3 film XRD test curve and Fe2O3 doping tungstic acid-nitrogen
Change the XRD test curve of carbon compound film)
Fig. 4 is that the tungstic acid of Fe2O3 doping prepared by the embodiment of the present invention 1-nitridation carbon compound film Raman tests map (certainly
It is upper and it is lower be respectively Fe2O3 doping WO 3 film Raman test curve, C3N4Raman test curve and Fe2O3 doping three aoxidize
Tungsten-nitridation carbon compound film Raman test curve.Fig. 4 b is Fig. 4 a 1050 to 1300cm-1The amplification in section is shown)
Fig. 5 is the tungstic acid of Fe2O3 doping prepared by the embodiment of the present invention 1-nitridation carbon compound film photo catalytic reduction Cr VI
Performance test figure
Specific embodiment
Technical solution of the present invention is described further below with reference to embodiment.
The present invention proposes a kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film, which is characterized in that described
Method is that Fe2O3 doping WO 3 film material is made using sodium tungstate and urea as raw material with hydro-thermal method in doping reagent with ferric nitrate
Material, by being impregnated in urea liquid, dry, calcining and etc. after, prepare Fe2O3 doping tungstic acid-carbonitride THIN COMPOSITE
Film, and include the following steps and content:
(1) raw material used by is commercially available sodium tungstate and ferric nitrate.
(2) preparation manipulation carries out under stirring.
(3) in preparation process, first a certain amount of sodium tungstate and ferric nitrate is dissolved in distilled water, stirred evenly, it then will be upper
It states and is slowly added to a certain amount of hydrochloric acid solution in solution, be vigorously stirred.
(4) FTO electro-conductive glass is added in the above solution, carries out hydro-thermal reaction, hydrothermal temperature is 80-200 DEG C, is protected
The warm time is 12-48 hours.
(5) after taking out the cleaning of FTO electro-conductive glass deionized water, 50-100 DEG C of vacuum drying.
(6) by above-mentioned FTO electro-conductive glass 300-800 DEG C temperature lower calcination 1-6 hours.
(7) above-mentioned gained Fe2O3 doping tungstic acid impregnated in urea liquid, take out drying, in 300-800 DEG C of temperature
Lower calcining 1-6 hours.
Obtained Fe2O3 doping tungstic acid-nitridation carbon compound film appearance is the uniform film in light yellow surface.
Under a scanning electron microscope, it may be observed that a large amount of irregular sheet-like particles, particle is about 4-5 microns.XRD test
Show that the film is collectively constituted by three oblique crystal phase tungstic acids and hexagonal phase tungstic acid.Point to be developed the color by sulfosalicylic acid
The content that light photometry measures iron in WO 3 film is between 0.3% to 5.0%.Three oxidations are obtained by XRD test analysis
The ratio of three oblique crystal phases and hexagonal phase is in 1:4 between 3:5 in W film.Meanwhile it being tested by Raman and showing the laminated film
There is C in sample3N4, testing its content by gravimetric method is about 0.01% to 0.5%.
In short, Fe2O3 doping tungstic acid-nitridation carbon compound film can be made using this technology.
Embodiment: being slowly dissolved in 300mL distilled water for the sodium tungstate of 23.1g under stirring, continues to stir
The ferric nitrate of 1% to the 50% different quality ratio relative to sodium tungstate is added in 30min while stirring, and FTO is added in the solution and leads
After electric glass, carried out hydro-thermal reaction 12-48 hours at 80-200 DEG C, after taking out the cleaning of FTO electro-conductive glass deionized water, 50-
100 DEG C of vacuum drying, obtain Fe2O3 doping WO 3 film in temperature lower calcination 1-6 hours at 300-800 DEG C；It is dipped in urea
Impregnate 10-60 minutes in saturated solution, 50-100 DEG C of vacuum drying, 300-800 DEG C temperature lower calcination 1-6 hours.
Prepared Fe2O3 doping tungstic acid-nitridation carbon compound film be it is light yellow, to heavy metal in water removal reaction before
Afterwards, pattern is basically unchanged (see Fig. 1), under scanning electron microscope, it may be observed that a large amount of irregular sheet-like particles, particle is about 4-
5 microns (see Fig. 2), which (is tested by compound form of three oblique crystal phases and hexagonal phase tungstic acid and C3N4 see XRD in Fig. 3
Figure illustrates in the film sample that Fig. 4 Raman test chart illustrates the film sample there are three oblique crystal phases and hexagonal phase tungstic acid
In have the carbonitride of C3N4 form, wherein Fig. 4 (b) is that the amplification in ordinate 1050 to the section 1300cm-1 in Fig. 4 (a) is shown,
Indicate C3N4 presence), there is excellent elimination performance to heavy metal Cr VI in water, within 90 minutes time, to 10mg/L six
Valence chromium solution photo catalytic reduction rate reaches 99.9% (see Fig. 5).
Claims (10)
1. a kind of Fe2O3 doping tungstic acid-nitridation carbon compound film, which is characterized in that the laminated film adulterates ferro element, should
Laminated film is by three oblique crystal phase tungstic acids, hexagonal phase tungstic acid and carbonitride C3N4Compound composition.
2. Fe2O3 doping tungstic acid-nitridation carbon compound film as described in claim 1, wherein the mass percent of iron is 0.3%
To between 5.0%.
3. Fe2O3 doping tungstic acid-nitridation carbon compound film as described in claim 1, wherein three oblique crystal phases and three oxygen of hexagonal phase
The ratio for changing tungsten is 1:4 between 3:5.
4. Fe2O3 doping tungstic acid-nitridation carbon compound film as described in claim 1, microstructure are shown with 4-5 microns
Particle.
5. Fe2O3 doping tungstic acid-nitridation carbon compound film as described in claim 1, wherein carbonitride C3N4Mass percent
Between 0.01% to 0.5%.
6. a kind of Fe2O3 doping tungstic acid-nitridation carbon compound film, the laminated film is Fe2O3 doping three described in claim 1
Tungsten oxide-nitridation carbon compound film, which is characterized in that the preparation method comprises the following steps:
(1) sodium tungstate and ferric nitrate are dissolved in distilled water, are stirred evenly；
(2) FTO glass substrate is added in the above solution, carries out hydro-thermal reaction；
(3) aforesaid substrate is taken out, calcines, forms WO 3 film on the substrate.
(4) WO 3 film is immersed into saturation urea liquid, by drying, calcining, forms Fe2O3 doping tungstic acid-nitridation
Carbon compound film.
7. the preparation method of laminated film as claimed in claim 6, wherein in the step (1), sodium tungstate is first added, then
The ferric nitrate for accounting for that the mass ratio of sodium tungstate is 1% to 50% is added.
8. the preparation method of laminated film as claimed in claim 6, wherein in the step (2), the temperature of hydro-thermal reaction is
80-200 DEG C, soaking time is 12-48 hours.
9. the preparation method of laminated film as claimed in claim 6, wherein in the step (3), the temperature range of calcining is
300-800 DEG C, calcination time is 1-6 hours.
10. the preparation method of laminated film as claimed in claim 6, wherein in the step (4), the temperature range of calcining
It is 300-800 DEG C, calcination time is 1-6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810900409.7A CN108993572A (en) | 2018-08-09 | 2018-08-09 | A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810900409.7A CN108993572A (en) | 2018-08-09 | 2018-08-09 | A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108993572A true CN108993572A (en) | 2018-12-14 |
Family
ID=64596475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810900409.7A Pending CN108993572A (en) | 2018-08-09 | 2018-08-09 | A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108993572A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981213A (en) * | 2019-12-18 | 2020-04-10 | 济南大学 | Preparation method of crossed plate-shaped tungsten trioxide-ferric oxide composite material |
| CN114514979A (en) * | 2020-11-19 | 2022-05-20 | 中国农业科学院油料作物研究所 | Green method for reducing aflatoxin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950253A (en) * | 2008-09-16 | 2014-07-30 | 株式会社东芝 | Hydrophilic films and components and structures using same |
| CN106365465A (en) * | 2016-08-29 | 2017-02-01 | 济南大学 | Preparation method of three-dimensional titanium dioxide-gold-carbon nitride ternary material |
-
2018
- 2018-08-09 CN CN201810900409.7A patent/CN108993572A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950253A (en) * | 2008-09-16 | 2014-07-30 | 株式会社东芝 | Hydrophilic films and components and structures using same |
| CN106365465A (en) * | 2016-08-29 | 2017-02-01 | 济南大学 | Preparation method of three-dimensional titanium dioxide-gold-carbon nitride ternary material |
Non-Patent Citations (2)
| Title |
|---|
| MINGCHAO FENG等: "The preparation of Fe doped triclinic-hexagonal phase heterojunction WO3 film and its enhanced photocatalytic reduction of Cr (VI)", 《MATERIALS RESEARCH BULLETIN》 * |
| YIPENG ZANG等: "Facile synthesis of composite g-C3N4/WO3: a nontoxic photocatalyst with excellent catalytic activity under visible light", 《RSC ADVANCES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981213A (en) * | 2019-12-18 | 2020-04-10 | 济南大学 | Preparation method of crossed plate-shaped tungsten trioxide-ferric oxide composite material |
| CN114514979A (en) * | 2020-11-19 | 2022-05-20 | 中国农业科学院油料作物研究所 | Green method for reducing aflatoxin |
| CN114514979B (en) * | 2020-11-19 | 2024-03-29 | 中国农业科学院油料作物研究所 | Green method for reducing aflatoxin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Cheng et al. | Structural, morphological, optical and photocatalytic properties of Gd-doped TiO2 films | |
| Wang et al. | High-efficiency visible-light AgI/Ag/Bi 2 MoO 6 as a Z-scheme photocatalyst for environmental applications | |
| Xiong et al. | Tailoring morphology, enhancing magnetization and photocatalytic activity via Cr doping in Bi25FeO40 | |
| CN109806776A (en) | Mix the method for the modified microfiltration membranes of iron graphene oxide titanic oxide nano compound material | |
| CN104437589A (en) | Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof | |
| CN102794186B (en) | Oxyhalide photo-catalytic material and preparation method thereof | |
| Qian et al. | Deep insight into the photocatalytic activity and electronic structure of amorphous earth-abundant MgAl 2 O 4 | |
| CN103372424B (en) | A kind of synthetic method of high activity N-F codope pucherite visible-light photocatalysis material | |
| CN105879871A (en) | Method for preparing plasma gold nanorod composite photocatalytic material with butterfly wing structure | |
| CN110479341A (en) | A kind of hydrogenation modification pucherite/class graphite phase carbon nitride composite photo-catalyst and preparation method thereof | |
| Sun et al. | Crystallinity and photocatalytic properties of BiVO4/halloysite nanotubes hybrid catalysts for sunlight-driven decomposition of dyes from aqueous solution | |
| Zhang et al. | Improved photocatalytic activities of porous In2O3 with large surface area by coupling with K-modified CuO for degrading pollutants | |
| CN108993572A (en) | A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film | |
| Uzunova-Bujnova et al. | Lanthanide-doped titanium dioxide layers as photocatalysts | |
| Guo et al. | 2D-Bi2MoO6/2D-g-C3N4 nanosheet heterojunction composite: synthesis and enhanced visible light photocatalytic mechanism | |
| Kang et al. | Hydrothermal synthesis of graphene-ZnTiO 3 nanocomposites with enhanced photocatalytic activities | |
| Wei et al. | A stable and efficient La-doped MIL-53 (Al)/ZnO photocatalyst for sulfamethazine degradation | |
| CN109395713B (en) | Cerium-titanium-doped bismuth tantalate niobate photocatalytic material and preparation method and application thereof | |
| CN105478153A (en) | CeVO4 / Ag / g-C3N4 composite photocatalyst and preparation method thereof | |
| Mishra et al. | Studying the Effects of Cu Doping on Structure and Photoluminescence Properties of SnO2 Nanoparticle with Its Effectiveness towards the Mineralization of Toxic Industrial Dye | |
| CN108772053B (en) | Bismuth titanate/bismuth oxide photocatalyst and preparation method and application thereof | |
| CN111389421B (en) | Preparation method and application of two-dimensional layered bismuth oxychloride and titanium niobate composite photocatalytic material | |
| CN111617784A (en) | Preparation method and application of two-dimensional layered bismuth oxychloride-Fe doped modified photocatalytic material | |
| CN110993355A (en) | Preparation method of optimized α -phase iron oxide photo-anode with two-dimensional titanium carbide substrate layer | |
| Ghorai et al. | Effect of photocatalytic activities of nano-sized copper molybdate (CuMoO4)-doped bismuth titanate (Bi2Ti4O11)(CMBT) alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181214 |