CN109300700A - A kind of preparation method of Fe2O3 doping bismuth tungstate - Google Patents
A kind of preparation method of Fe2O3 doping bismuth tungstate Download PDFInfo
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- CN109300700A CN109300700A CN201810942588.0A CN201810942588A CN109300700A CN 109300700 A CN109300700 A CN 109300700A CN 201810942588 A CN201810942588 A CN 201810942588A CN 109300700 A CN109300700 A CN 109300700A
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- bismuth tungstate
- distilled water
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 58
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 58
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 50
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012153 distilled water Substances 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 239000000376 reactant Substances 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 13
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000010668 complexation reaction Methods 0.000 claims abstract description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 150000001805 chlorine compounds Chemical class 0.000 claims abstract description 6
- -1 tungstate dihydrate Chemical class 0.000 claims abstract description 6
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 206010013786 Dry skin Diseases 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 235000017550 sodium carbonate Nutrition 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 229940001593 sodium carbonate Drugs 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 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
- 239000011734 sodium Substances 0.000 abstract description 4
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000004809 Teflon Substances 0.000 description 6
- 229920006362 Teflon® Polymers 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 241000446313 Lamella Species 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 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 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 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
- 150000004767 nitrides Chemical class 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of Fe2O3 doping bismuth tungstate, comprising the following steps: five water bismuth nitrates is added in the aqueous solution containing citric acid to form metal-citrate complexation object.It is vigorously stirred after ten minutes, tungstate dihydrate acid sodium is added and sodium bicarbonate is added in above-mentioned solution.It futher stirs after five minutes, compactedness is 50% in a kettle, is cooled to room temperature after keeping the temperature 15 hours at a temperature of 180 DEG C；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, obtain flower-shaped bismuth tungstate material.The DMF and distilled water that volume ratio is 8:2 are measured, mixed solvent is used as after mixing；Above-mentioned bismuth tungstate and four water frerrous chlorides are added in mixed solvent.It is futher stirring after five minutes, compactedness is 50% in a kettle, is cooled to room temperature after keeping the temperature 2 hours at a temperature of 100 DEG C；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, obtain Fe2O3 doping bismuth tungstate material.
Description
Technical field
The invention belongs to field of material technology, devise a kind of preparation method of Fe2O3 doping bismuth tungstate material.Production preparation
The material has use value in stored energy application, energy conservation and environmental protection.
Background technique
Supercapacitor or supercapacitor are recently due to its high power density (1-10 kilowatt/kilogram) than conventional batteries system
System (150 watt/kilogram) obtains more and more interest.These charge storages in electrode/electrolyte interface and outer surface, and
It is not electrode volume, this is conducive to fast charge/discharge rate, this is the main original that supercapacitor has high power density
Cause.In addition, biometrics will at 100,000 times or so, and supercapacitor have the longer shelf-life, high efficiency, environmental protection and make
With safety.The main application of this supercapacitor includes hybrid-electric car, they are used together with battery.Other application packet
Include mobile phone, camera, UPS (uninterruptible power supply), braking energy system etc..The major defect of these capacitors is its energy density
It is low.The possibility mode that energy density (being provided by 1/2CV2) can be modified is (i) by increasing specific capacitance or (ii) increase material
Cell voltage.Specific capacitance with the amount of the energy of unit mass/volume (energy density) storage by electrode material, the electricity of electrode
Son/ionic conductivity and the ionic conductivity and stability window of electrolyte determine.
Based on charge-storage mechanism, supercapacitor is divided into two types, such as double layer capacitor (EDLC) and pseudo-capacitance
Device.In EDLC, charge is stored by adsorption/desorption process.Carbon-based material such as activated carbon, carbon aerogels and carbon nanotube by with
Make EDLC electrode.On the other hand, in pseudo-capacitance, charge is stored by faraday's reaction.Transition metal oxide and conduction are poly-
It closes object and is widely used as electrode.Compared with EDLC, these pseudo-capacitances have higher energy density since capacitor increases.Cause
This, is using transition metal oxide, the active electrode of hydroxide and nitride as pseudo-capacitance device.
Bismuth tungstate is a kind of excellent functional material.Bismuth tungstate has piezoelectricity, thermoelectricity, ferroelectricity, nonlinear dielectric magnetization
Rate, catalysis and oxide anion conduct behavior.They are used as excellent visible-light photocatalyst, for degradation of contaminant and
Organic dyestuff, the electrode material of lithium ion battery and for water decomposition oxygen and the reaction of hydrogen etc..Bismuth tungstate is due to having
Multiple reaction center Bi+3And WO6 +6, theoretical capacity is high, and the large specific surface area of sheet bismuth tungstate can come into full contact with electrolyte,
But its electric conductivity is poor.
The present invention uses the flower-shaped bismuth tungstate material of solvent structure, then by above-mentioned material and four water frerrous chloride solvent heats
Method synthesizes Fe2O3 doping bismuth tungstate material, and the doping of iron can improve the electric conductivity of bismuth tungstate to improve chemical property.
Summary of the invention
The present invention is directed to the middle deficiency of the prior art, proposes a kind of preparation method of Fe2O3 doping bismuth tungstate.Solution of the present invention
Certainly the technical issues of is that citric acid method is added in hydrothermal reaction process, metal-citrate complexation object is formed, then rear
Temperature raising can uniformly release ion under the conditions of continuous solvent heat, while sodium bicarbonate is added and adjusts PH, ultimately form
Laminated structure stereo stocking is at flower-like structure.The flower-shaped bismuth tungstate diameter of preparation is in 20um.Second step is by by ferro element
Flower-shaped bismuth tungstate material internal is added to increase conductive and capacitance.
A kind of preparation method of Fe2O3 doping bismuth tungstate material, comprising the following steps:
Step 1: it weighs molar ratio and is dissolved in distilled water aqueous solution for the five water bismuth nitrates and citric acid of 1:1 to be formed
The metal of 0.5mol/L-citrate complexation object；It is vigorously stirred after ten minutes, obtains solution A.
Step 2: it weighs molar ratio and is added in solution A for the tungstate dihydrate acid sodium and sodium bicarbonate of 1:4.Further stirring
It mixes after five minutes, and is cooled to room temperature after solvent thermal reaction 10-15 hours at a temperature of 180 DEG C；Take out reactant alcohol and steaming
Distilled water carries out eccentric cleaning each 3 times, and 70 DEG C are arrived flower-shaped bismuth tungstate material in drying 12 hours；Wherein five water in step 1 and step 2
Bismuth nitrate, citric acid, tungstate dihydrate acid sodium and sodium bicarbonate molar ratio be 2:2:1:4；
Step 3: the DMF and distilled water that volume ratio is 8:2 are measured, mixed solvent, the two volume and conduct are used as after mixing
Mixed solvent volume is for calculating；
Obtained flower-shaped bismuth tungstate material and four water frerrous chlorides are added to above-mentioned mixed solvent；Obtained mixed solution
Concentration be 0.175-0.225mol/L；Wherein flower-shaped bismuth tungstate material and four water frerrous chlorides are 5:2~5:4 in molar ratio；
It is vigorously stirred after ten minutes, is cooled to room temperature within solvent thermal reaction 2 hours at a temperature of 100 DEG C；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping tungsten in 12 hours
Sour bismuth material.
Compared with the existing technology, beneficial effects of the present invention are as follows:
(1) the flower-shaped bismuth tungstate of use has the characteristics that prepare simple as substrate, and structure is stood by multiple lamellar structures
Body is accumulated to be formed, and surface area ratio is larger, to increase the contact area with electrolyte, electric double layer capacitance effect can be improved.Together
When, it can reduce the diffusion length of carrier, to reduce the internal resistance of electrode.
(2) the method for the present invention simple process is easy to control, and is convenient for industrialized production.Obtained composite material is in energy storage
Using having use value in, energy conservation and environmental protection.
(3) the part bismuth in the bismuth tungstate of part is replaced by ferro element and reaches increase electric conductivity and capacity effect.
(4) so that more smooth lamellar structure is become porous lamellar structure in this way by addition ferro element solvent thermal reaction has
Conducive to increase capacity effect.
Detailed description of the invention
Fig. 1 is the step flow chart of the preparation method of the Fe2O3 doping bismuth tungstate material of the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the bismuth tungstate of the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope of the Fe2O3 doping bismuth tungstate material of the embodiment of the present invention 3；
Fig. 4 is the bismuth tungstate of the embodiment of the present invention 3 and the XRD diagram of Fe2O3 doping bismuth tungstate material；
Fig. 5 is the CV figure under supercapacitor different scanning speed prepared by the bismuth tungstate of the embodiment of the present invention 3；
Fig. 6 is under supercapacitor different scanning speed prepared by the Fe2O3 doping bismuth tungstate material of the embodiment of the present invention 3
CV figure；
Fig. 7 is the high rate performance figure under supercapacitor difference current density prepared by the bismuth tungstate of the embodiment of the present invention 3；
Fig. 8 is under supercapacitor difference current density prepared by the Fe2O3 doping bismuth tungstate material of the embodiment of the present invention 3
High rate performance figure.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carry out clearly, it is complete
Site preparation description, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.Based on this hair
Embodiment in bright, those of ordinary skill in the art under the premise of not making creative work achievement it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
Referring to Fig. 1, it show a kind of step process of the preparation method of Fe2O3 doping bismuth tungstate material of the embodiment of the present invention
Figure comprising following steps:
S10 weighs molar ratio and is dissolved in 10mL distilled water for the five water bismuth nitrates and citric acid of 1:1 to form metal-lemon
Lemon hydrochlorate complex compound.It is vigorously stirred after ten minutes, obtains mixed solution, mixed liquor volume is for calculating；
S20 weighs the solution A that molar ratio is dissolved in 10mL for the tungstate dihydrate acid sodium and sodium bicarbonate of 1:4.Further stir
After five minutes, it is cooled to room temperature after solvent thermal reaction；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C
Obtain flower-shaped bismuth tungstate material within dry 12 hours.
Bi in the above reaction+3Metal complex is formed with the in the mixed solvent of citric acid.Bi+3In solvent heat process conditions
Under slowly unlock complex status and WO6 -6Reaction forms Bi2WO6, wherein sodium bicarbonate be used for in citric acid and maintain PH put down
Weighing apparatus.
It, can be further by Fe on the basis of bismuth tungstate is prepared in above step+2It reacts to form Fe2O3 doping wolframic acid
Bismuth material.
S30 measures DMF and distilled water that volume ratio is 8:2, as mixed solvent, the two volume and as mixed after mixing
Bonding solvent volume is for calculating；
S40, the flower-shaped Bi that will be obtained2WO6Material and four water frerrous chlorides are that 5:2~5:4 is added to above-mentioned mix in molar ratio
Bonding solvent.It is vigorously stirred after ten minutes, is cooled to room temperature after solvent thermal reaction；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping tungsten in 12 hours
Sour bismuth material.
Illustrate implementation process of the invention below by way of several concrete application embodiments.
Embodiment 1
S10, by 0.25mmol Bi (NO3)3·5H2O be added in the 10mL aqueous solution containing 0.25mmol citric acid with
Form metal-citrate complexation object.It is vigorously stirred after ten minutes, obtains solution A.
0.125mmol Na is added in S202WO4·2H2O and 0.5mmol NaHCO3It is added in above-mentioned solution.Into one
Step stirring after five minutes, solution is poured into the stainless steel autoclave of the Teflon lining with 20mL capacity, and in 180 DEG C of temperature
Degree is cooled to room temperature after lower heat preservation 15 hours；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings
Obtain within 12 hours flower-shaped bismuth tungstate material.
It is piled into well by the more smooth lamella of the flower-shaped bismuth tungstate of 2um-5um that Fig. 2 observes above step preparation flower-shaped
Structure, such surface area ratio is larger, convenient for the progress of next step.
S30 measures DMF and distilled water that volume ratio is 8:2, as mixed solvent, the two volume and as mixed after mixing
Bonding solvent volume is for calculating；
S40, by the flower-shaped bismuth tungstate material of obtained 0.125mmol and 0.1mmolFeCl2·4H2O is added to above-mentioned mixing
Solvent (10mL).It is vigorously stirred after ten minutes, solution is poured into the stainless steel autoclave of the Teflon lining with 20mL capacity
In, and be cooled to room temperature after keeping the temperature 2 hours at a temperature of 100 DEG C；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping tungsten in 12 hours
Sour bismuth material.
Embodiment 2
S10, by 0.25mmol Bi (NO3)3·5H2O be added in the 10mL aqueous solution containing 0.25mmol citric acid with
Form metal-citrate complexation object.It is vigorously stirred after ten minutes, obtains solution A.
0.125mmol Na is added in S202WO4·2H2O and 0.5mmol NaHCO3It is added in above-mentioned solution.Into one
Step stirring after five minutes, solution is poured into the stainless steel autoclave of the Teflon lining with 20mL capacity, and in 180 DEG C of temperature
Degree is cooled to room temperature after lower heat preservation 12 hours；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings
Obtain within 12 hours flower-shaped bismuth tungstate material.
S30 measures DMF and distilled water that volume ratio is 8:2, as mixed solvent, the two volume and as mixed after mixing
Bonding solvent volume is for calculating；
S40, by the flower-shaped bismuth tungstate material of obtained 0.125mmol and 0.07mmol
FeCl2·4H2O is added to above-mentioned mixed solvent (10mL).It is vigorously stirred after ten minutes, solution, which is poured into, to be had
In the stainless steel autoclave of the Teflon lining of 20mL capacity, and it is cooled to room temperature after keeping the temperature 2 hours at a temperature of 100 DEG C；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping tungsten in 12 hours
Sour bismuth material.
Embodiment 3
S10, by 0.25mmol Bi (NO3)3·5H2O be added in the 10mL aqueous solution containing 0.25mmol citric acid with
Form metal-citrate complexation object.It is vigorously stirred after ten minutes, obtains solution A.
0.125mmol Na is added in S202WO4·2H2O and 0.5mmol NaHCO3It is added in above-mentioned solution.Into one
Step stirring after five minutes, solution is poured into the stainless steel autoclave of the Teflon lining with 20mL capacity, and in 180 DEG C of temperature
Degree is cooled to room temperature after lower heat preservation 10 hours；It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings
Obtain within 12 hours flower-shaped bismuth tungstate material.
It is piled into well by the more smooth lamella of the flower-shaped bismuth tungstate of 2um-5um that Fig. 2 observes above step preparation flower-shaped
Structure, such surface area ratio is larger, convenient for the progress of next step.
S30 measures DMF and distilled water that volume ratio is 8:2, as mixed solvent, the two volume and as mixed after mixing
Bonding solvent volume is for calculating；
S40, by the flower-shaped bismuth tungstate material of obtained 0.125mmol and 0.05mmol FeCl2·4H2O is added to above-mentioned mixed
Bonding solvent (10mL).It is vigorously stirred after ten minutes, solution is poured into the stainless steel high pressure of the Teflon lining with 20mL capacity
In kettle, and it is cooled to room temperature after keeping the temperature 2 hours at a temperature of 100 DEG C；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping tungsten in 12 hours
Sour bismuth material.
Referring to Fig. 3 it can be seen that diameter is the Fe2O3 doping bismuth tungstate material of 2um-5um, the flower-shaped bismuth tungstate in part is also retained
Structure, and porous lamella is converted by original smooth lamella, be conducive to enhance capacity effect in this way.Pass through the XRD of Fig. 4
Figure is it can be seen that Bi1.5Fe0.5WO6Peak illustrate Fe+3Part Bi is substituted+3, can see and pass through by the comparison of Fig. 5 and Fig. 6
The area of CV after replacement obviously becomes larger.It can see high rate performance by the comparison of Fig. 7 and Fig. 8 also to improve.
The foregoing is merely preferred embodiments of the invention, be not intended to limit the present invention, it is all spirit of that invention and principle with
Within interior done any modification, improvement etc. all belong to the scope of protection of the present invention.
Claims (1)
1. a kind of preparation method of Fe2O3 doping bismuth tungstate, which is characterized in that this method specifically includes the following steps:
Step 1: it weighs molar ratio and is dissolved in distilled water aqueous solution for the five water bismuth nitrates and citric acid of 1:1 to form 0.5mol/
The metal of L-citrate complexation object；It is vigorously stirred after ten minutes, obtains solution A；
Step 2: it weighs molar ratio and is added in solution A for the tungstate dihydrate acid sodium and sodium bicarbonate of 1:4；Futher stirring 5 points
Zhong Hou, and be cooled to room temperature after solvent thermal reaction 10-15 hours at a temperature of 180 DEG C；Take out reactant alcohol and distilled water
It carries out eccentric cleaning each 3 times, 70 DEG C are arrived flower-shaped bismuth tungstate material in drying 12 hours；Wherein five water nitric acid in step 1 and step 2
Bismuth, citric acid, tungstate dihydrate acid sodium and sodium bicarbonate molar ratio be 2:2:1:4；
Step 3: the DMF and distilled water that volume ratio is 8:2 are measured, as mixed solvent, the two volume and as mixing after mixing
Solvent volume is for calculating；
Obtained flower-shaped bismuth tungstate material and four water frerrous chlorides are added to above-mentioned mixed solvent；Obtained mixed solution it is dense
Degree is 0.175-0.225mol/L；Wherein flower-shaped bismuth tungstate material and four water frerrous chlorides are 5:2~5:4 in molar ratio；Acutely
Stirring after ten minutes, is cooled to room temperature for solvent thermal reaction 2 hours at a temperature of 100 DEG C；
It takes out reactant alcohol and distilled water carries out eccentric cleaning each 3 times, 70 DEG C of dryings obtain Fe2O3 doping bismuth tungstate in 12 hours
Material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS553302A (en) * | 1978-03-31 | 1980-01-11 | Kouichirou Sakata | Magnetic capacitor material |
| CN102500390A (en) * | 2011-11-17 | 2012-06-20 | 陕西科技大学 | Preparation method of iron oxide/bismuth tungstate composite photocatalyst |
| CN107162059A (en) * | 2017-06-13 | 2017-09-15 | 浙江大学 | One kind prepares sheet Bi2WO6Method |
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2018
- 2018-08-17 CN CN201810942588.0A patent/CN109300700B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS553302A (en) * | 1978-03-31 | 1980-01-11 | Kouichirou Sakata | Magnetic capacitor material |
| CN102500390A (en) * | 2011-11-17 | 2012-06-20 | 陕西科技大学 | Preparation method of iron oxide/bismuth tungstate composite photocatalyst |
| CN107162059A (en) * | 2017-06-13 | 2017-09-15 | 浙江大学 | One kind prepares sheet Bi2WO6Method |
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| Title |
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| 许雪棠等: "Fe/Bi2WO6水热合成及其光催化性能研究", 《无机盐工业》 * |
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