CN106268844A - A kind of preparation method of photocatalyst bismuth ferrite - Google Patents
A kind of preparation method of photocatalyst bismuth ferrite Download PDFInfo
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- CN106268844A CN106268844A CN201610668680.3A CN201610668680A CN106268844A CN 106268844 A CN106268844 A CN 106268844A CN 201610668680 A CN201610668680 A CN 201610668680A CN 106268844 A CN106268844 A CN 106268844A
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- bismuth ferrite
- photocatalyst
- xerogel
- colloidal sol
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 49
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 41
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 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 abstract description 14
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 11
- 239000011975 tartaric acid Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 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
- 229910002902 BiFeO3 Inorganic materials 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 238000010668 complexation reaction Methods 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000002738 chelating agent Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000003980 solgel method Methods 0.000 description 6
- 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 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IUOOGQJPAJDLFV-UHFFFAOYSA-N 2,3-dihydroxybutanedioic acid;ethane-1,2-diol Chemical compound OCCO.OC(=O)C(O)C(O)C(O)=O IUOOGQJPAJDLFV-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910002897 Bi2Fe4O9 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007775 ferroic material Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- B01J35/39—
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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 invention discloses the preparation method of a kind of photocatalyst bismuth ferrite, it is characterised in that comprise the following steps: by bismuth nitrate and ferric nitrate according to BiFeO3The proportioning of chemical formula is dissolved in salpeter solution, and adds the tartaric acid as chelating agent and ethylene glycol stirring and dissolving；Described mixed solution is heated to 80 DEG C, obtains colloidal sol, and described colloidal sol is dried at 120 DEG C, obtain xerogel；Calcine after grinding described xerogel, obtain described photocatalyst bismuth ferrite.The preparation method of photocatalyst bismuth ferrite provided by the present invention has the advantages such as reaction temperature is low, course of reaction is easily controllable, and the uniformity of goods, purity are high, stoichiometry is accurate, preparation process is simple, preparation cost is cheap.
Description
Technical field
The present invention relates to photocatalysis technology field, particularly relate to a kind of photocatalyst bismuth ferrite utilizing sol-gel process
Simple preparation method.
Background technology
Along with energy scarcity and problem of environmental pollution increasingly sharpen, photocatalysis technology is in hydrogen production by water decomposition and organic contamination
The fields such as thing degraded have broad application prospects, and are to solve the energy and a kind of ideal green technology of environmental problem, titanium dioxide
Titanium has advantages such as high, stable, the non-secondary pollution of catalytic efficiency as widely used photocatalyst, but its greater band gap (～
3.2eV), only the ultraviolet light accounting for solar energy about 5% being had response, solar energy utilization ratio is relatively low.Based on this, people couple
TiO2Carry out a large amount of study on the modification, to improve its visible light catalysis activity, continually develop new semiconductor light-catalyst simultaneously.
Recently, the photocatalysis performance of bismuth ferrite attracts attention.It is a kind of common multi-ferroic material, always condensed state
Physics and the study hotspot of material science, it has narrower band gap (～2.0eV), is suitable to absorb visible ray, therefore ferrum
Acid bismuth is also a kind of potential visible light catalytic material.The physical property of material is with its pattern, dimension, size and defect etc. closely
Relevant, the especially photocatalyst of nanoscale can show the photocatalytic activity of enhancing.The method of preparation nano material is very
Many.Solid reaction process is used to synthesize bismuth ferrite, according to Bi2O3-Fe2O3Phasor, if the Bi of high temperature mixing2O3-Fe2O3Delay with stove
Slow cool down, then except generating BiFeO3Outside principal phase, also can form other dephasign containing Fe, Bi.If with Bi2O3、Fe2O3For bismuth source
And source of iron, then use NaNO3And KNO3Composite fused salt method Fast back-projection algorithm bismuth ferrite powder.When temperature of molten salt is 500 DEG C, Bi2O3With
Fe2O3Between start reaction generate Bi25FeO40Phase, when temperature of molten salt is increased to 600 DEG C, starts to generate a small amount of bismuth ferrite fused salt；Temperature
When degree continues to bring up to 650 DEG C and 700 DEG C, nearly all form pure phase bismuth ferric, but still have trace dephasign Bi25FeO40With
Bi2Fe4O9。
Wherein sol-gel process synthesis is one of most important method preparing nano material at present.Sol-gel process
Feature is: be raw material with liquid chemical reagent or colloidal sol, the raw reaction of reactant uniform hybrid concurrency under liquid phase, generates stable
Sol, is changed into gel after placing certain time, wherein contains a large amount of liquid phase, can remove liquid medium by evaporation.Colloidal sol-
It is low that gel method has reaction temperature, and course of reaction is easily controllable；The uniformity of goods, purity are high, and (uniformity is up to molecule or former
Sub-level)；The advantages such as stoichiometry is accurate, it is easy to modified, the wide ranges (including amount and the kind of doping) of doping.But the most also
There are some drawbacks, the process means that the xerogel that its unstability causes different solvents and preparation flow to obtain is used are also
Can have nothing in common with each other, therefore a series of research will be carried out for these factors.
It addition, heat treating process is always the important means of adjusting seed size size, but along with the rising of annealing temperature, crystal grain leads to
Often it is difficult to uniformly grow up simultaneously, and because being limited by materials synthesis temperature, it is impossible to obtained by the method reducing annealing temperature
Obtain smaller nano-particle.Therefore, use the tartaric acid-ethylene glycol sol-gal process of improvement herein, added by regulation
Tartaric acid-ethylene glycol consumption, prepare the bismuth ferrate nano granule of size tunable, and under visible light exposure, test photocatalysis fall
Solve the reactivity worth of methyl orange.
(1) ferrum can be tentatively concluded that by the investigation of the report of bismuth ferrite material being prepared by sol-gel process
The acid final synthesis temperature of bismuth is the most all higher than 400 DEG C, is concentrated mainly between 500-650 DEG C；(2) use nitrate as metal
Ion source, and Bi excess can prevent the volatilization of Bi in roasting process under normal circumstances, if whole proportioning, finally produces
Thing often occurs impurity phase；(3) impurity in end product communicates the way removing cleaned frequently with dust technology.
Accordingly, it would be desirable to a kind of method of simpler low cost prepares photocatalyst bismuth ferrite.
Summary of the invention
For solving problem above, the present invention proposes the preparation method of a kind of novel photocatalyst bismuth ferrite, and its feature exists
In comprising the following steps: (1) by bismuth nitrate and ferric nitrate according to BiFeO3The proportioning of chemical formula is dissolved in salpeter solution, and
Add the tartaric acid as chelating agent and ethylene glycol stirring and dissolving；(2) the described mixed solution in step (1) is heated to 80
DEG C, obtain colloidal sol, and described colloidal sol is dried at 120 DEG C, obtain xerogel；(3) described the doing in grinding steps (2) is coagulated
Calcine after glue, obtain described photocatalyst bismuth ferrite.
Advantageously, the mol ratio of the bismuth nitrate in step (1) and ferric nitrate is 1.3:1.
Advantageously, the chelating agent in step (1) is 2.5:1 with the mol ratio of metal cation.
Advantageously, the mol ratio of the tartaric acid in step (1) and ethylene glycol is 1:18.
Advantageously, the stirring in step (1) is to utilize magnetic agitation.
Advantageously, the dry described colloidal sol in step (2) includes being placed in thermostatic drying chamber by described colloidal sol, 120
It is dried 24 hours at DEG C, obtains xerogel.
Advantageously, grinding in step (3) and calcine described xerogel and include described xerogel is ground to form fine powder, put
Enter crucible to be inserted in tube furnace and calcine 3 hours at 450 DEG C-600 DEG C.
The preparation method of photocatalyst bismuth ferrite provided by the present invention has that reaction temperature is low, course of reaction is prone to control
System, the advantages such as the uniformity of goods, purity are high, stoichiometry is accurate, preparation process is simple, preparation cost is cheap.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, also may be used
To obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the schematic flow diagram of the preparation method of the photocatalyst bismuth ferrite that the embodiment of the present invention provides.
Specific embodiment
Make to describe in more detail further to technical scheme with specific embodiment below in conjunction with the accompanying drawings.Obviously,
Described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the reality in the present invention
Execute example, the every other embodiment that those of ordinary skill in the art are obtained on the premise of not making creative work, all
The scope of protection of the invention should be belonged to.
It is an object of the invention to provide a kind of under visible ray the efficiency light that has of degradation water and organic pollution urge
Change bismuth ferrite photocatalyst of activity, nanoscale and preparation method thereof.The present invention uses sol-gel process to prepare bismuth ferrite,
Owing to bismuth ferrite has less energy band band gap, the bismuth ferrite material of nanostructured is as visible light catalyst, it is possible to realization has
The degraded of organic pollutants and hydrogen production by water decomposition.It is low that sol-gel process has reaction temperature, and course of reaction is easily controllable, goods
The uniformity, purity high (uniformity is up to molecule or atomic level), the stoichiometry advantage such as accurately, preparation process is simple, easily
In recycling, it is a kind of eco-friendly photocatalyst, and with low cost has good industrial prospect.
Fig. 1 is the schematic flow diagram of the preparation method of the photocatalyst bismuth ferrite that the embodiment of the present invention provides.Such as Fig. 1 institute
Showing, the preparation method of photocatalyst bismuth ferrite provided by the present invention comprises the following steps:
Step S102: by bismuth nitrate and ferric nitrate according to BiFeO3The proportioning of chemical formula is dissolved in salpeter solution.Treat molten
After liquid clarification, it is sequentially added into the tartaric acid as chelating agent and ethylene glycol stirring and dissolving.In one embodiment, bismuth nitrate and
The mol ratio of ferric nitrate is 1.3:1.In one embodiment, chelating agent is 2.5:1 with the mol ratio of metal cation.At one
In embodiment, the mol ratio of tartaric acid and ethylene glycol is 1:18.In one embodiment, above-mentioned stirring is to utilize magnetic agitation,
So that additive fully dissolves.
Step S104: after solution mix homogeneously, clarification, the described mixed solution in step S102 is heated to 80 DEG C,
Being allowed to occur heat polymerization, after several minutes, solution slowly transfers colloidal sol to, and is dried at 120 DEG C by described colloidal sol, obtains
Xerogel.In one embodiment, it is dried described colloidal sol to include: be placed in thermostatic drying chamber by described colloidal sol, at 120 DEG C
It is dried 24 hours, obtains xerogel.
Step S106: calcine after the described xerogel in grinding steps S104, obtains described photocatalyst bismuth ferrite.
In one embodiment, grind and calcine described xerogel to include: described xerogel is ground to form fine powder, puts in crucible and put
Enter in tube furnace at 450 DEG C-600 DEG C (such as, 450 DEG C, 500 DEG C, 550 DEG C, 600 DEG C) to calcine 3 hours.
As follows to the influence research of methyl orange degradation rate to bismuth ferrite particle size, the wherein initial concentration of methyl orange
10mg/L, bismuth ferrite consumption is 2.5g/L, and ultraviolet light irradiation time is 6 hours, it is seen that light irradiation time is 14 hours, bismuth ferrite
Nano-particle all shows good photocatalytic activity under ultraviolet light and visible light exposure, and along with the reduction of particle size
Its catalysis activity increases.When particle size is reduced to 52nm, respectively may be about at ultraviolet light and visible ray Methyl Orange degradation rate
71% and 39%.Along with the reduction of particle size, probability compound in vivo is reduced by the photo-generate electron-hole of generation, and electronics-
Hole to more can effective mobility to catalyst surface；And particle size is the least, specific surface area is the biggest, thus is light-catalyzed reaction
More available surface activity position is provided.
Advantageously, the preparation method of photocatalyst bismuth ferrite provided by the present invention is by adding the tartaric acid of different content
And ethylene glycol, use the mode controlling sintering temperature to be prepared for particle diameter regulatable bismuth ferrate nano granule, particle size distribution
Uniformly, granule-morphology is regular, and approximation is in spherical.Photocatalysis experiment prove: bismuth ferrate nano granule under visible light exposure to first
Base orange has good photocatalytic Degradation.Finding, particle size has considerable influence to the degradation rate of methyl orange simultaneously.Should
Result is that the photocatalytic applications of promotion bismuth ferrite is significant.
The preparation method of photocatalyst bismuth ferrite provided by the present invention contains with the relative of ethylene glycol by changing tartaric acid
Measure and regulate sintering temperature and be prepared for the bismuth ferrite nano powder of varying particle size.Tartaric acid and ethylene glycol rub with certain
That ratio (1:18), (such as, 450 DEG C, 500 DEG C, 550 DEG C, 600 DEG C) are calcined 3 hours at different temperatures.All samples is respectively formed
High-purity bismuth ferrite phase, occurs without other dephasign.If sintering temperature is too low, presoma degree of crystallinity can not get bismuth ferrite not
Crystal.If sintering temperature is too high, presoma carbonization is serious, and a large amount of dephasigns generate and have a strong impact on product property.
Note that ethylene glycol can regulate the characteristic of colloid, the especially size of colloid hole as polymerizer.Along with second
The increase of glycol content, colloid pore-size is gradually reduced, and this is the physical basis of regulation and control calcined product average grain size.But
It is that ethylene glycol content is unsuitable too much otherwise can cause xerogel hardening, and dephasign occurs in calcined product, and crystal grain also can become
Uneven.
Compared with traditional gel method, this patent with the addition of appropriate tartaric acid as chelating agent in precursor solution.
In gelinite dry run, tartaric acid takes the lead in because its carburizing temperature is relatively low carbonization, forms carbonaceous skeleton, thus effectively
Inhibit collapsing of gelinite, provide strong guarantee for obtaining high-quality bismuth ferrite nano powder.
The above disclosed preferred embodiment being only in the embodiment of the present invention, can not limit this with this certainly
Bright interest field, the equivalent variations therefore made according to the claims in the present invention, still belong to the scope that the present invention is contained.
Claims (7)
1. the preparation method of a photocatalyst bismuth ferrite, it is characterised in that comprise the following steps:
(1) by bismuth nitrate and ferric nitrate according to BiFeO3The proportioning of chemical formula is dissolved in salpeter solution, and adds as complexation
The tartaric acid of agent and ethylene glycol stirring and dissolving；
(2) the described mixed solution in step (1) is heated to 80 DEG C, obtains colloidal sol, and described colloidal sol is done at 120 DEG C
Dry, obtain xerogel；
(3) calcine after the described xerogel in grinding steps (2), obtain described photocatalyst bismuth ferrite.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that the nitric acid in step (1)
The mol ratio of bismuth and ferric nitrate is 1.3: 1.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that the complexation in step (1)
Agent is 2.5: 1 with the mol ratio of metal cation.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that the winestone in step (1)
The mol ratio of acid and ethylene glycol is 1:18.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that the stirring in step (1)
It is to utilize magnetic agitation.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that being dried in step (2)
Described colloidal sol includes being placed in thermostatic drying chamber described colloidal sol, is dried 24 hours, obtains xerogel at 120 DEG C.
The preparation method of photocatalyst bismuth ferrite the most according to claim 1, it is characterised in that the grinding in step (3)
And calcine described xerogel to include described xerogel is ground to form fine powder, put into crucible is inserted in tube furnace 450 DEG C-
Calcine 3 hours at 600 DEG C.
Priority Applications (1)
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| CN106698521A (en) * | 2017-02-27 | 2017-05-24 | 陕西科技大学 | Three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof |
| CN108786826A (en) * | 2018-06-15 | 2018-11-13 | 肇庆市华师大光电产业研究院 | A kind of solid-carrying type copper yttrium codope bismuth ferrite photocatalyst and its preparation method and application |
| KR20190069906A (en) | 2017-12-12 | 2019-06-20 | 울산대학교 산학협력단 | Photocatalyst containing Barium doped Bismuth ferrite, and water treatment method using the same |
| CN110451575A (en) * | 2019-09-11 | 2019-11-15 | 哈尔滨工业大学 | A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional effect |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698521A (en) * | 2017-02-27 | 2017-05-24 | 陕西科技大学 | Three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof |
| CN106698521B (en) * | 2017-02-27 | 2018-04-10 | 陕西科技大学 | A kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof |
| KR20190069906A (en) | 2017-12-12 | 2019-06-20 | 울산대학교 산학협력단 | Photocatalyst containing Barium doped Bismuth ferrite, and water treatment method using the same |
| CN108786826A (en) * | 2018-06-15 | 2018-11-13 | 肇庆市华师大光电产业研究院 | A kind of solid-carrying type copper yttrium codope bismuth ferrite photocatalyst and its preparation method and application |
| CN108786826B (en) * | 2018-06-15 | 2021-09-03 | 肇庆市华师大光电产业研究院 | Immobilized copper-yttrium co-doped bismuth ferrite photocatalyst and preparation method and application thereof |
| CN110451575A (en) * | 2019-09-11 | 2019-11-15 | 哈尔滨工业大学 | A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional effect |
| CN110451575B (en) * | 2019-09-11 | 2022-04-05 | 哈尔滨工业大学 | Method for enhancing magnetic property of bismuth ferrite nanopowder based on size effect |
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