CN102583566A - Preparation method for bismuth ferrate nano fibers - Google Patents
Preparation method for bismuth ferrate nano fibers Download PDFInfo
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- CN102583566A CN102583566A CN201110023191XA CN201110023191A CN102583566A CN 102583566 A CN102583566 A CN 102583566A CN 201110023191X A CN201110023191X A CN 201110023191XA CN 201110023191 A CN201110023191 A CN 201110023191A CN 102583566 A CN102583566 A CN 102583566A
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Abstract
The invention discloses a preparation method for bismuth ferrate nano fibers and aims to solve the technical problem that the traditional photocatalytic material has a wide band gap. The invention adopts the technical scheme which comprises the following steps of: dissolving citric acid in deionized water to form a citric acid solution; adding ferric nitrate and bismuth nitrate into the citric acid solution, stirring the mixture until the mixture is clear and transparent, after standing the solution, heating and stirring the solution in a water-bath pot, adding polyvinylpyrrolidone into the solution, continuously stirring until the polyvinylpyrrolidone is completely dissolved, keeping the concentration of the polyvinylpyrrolidone, performing electrostatic spinning by using an injection pump and a high-pressure power supply, and collecting the fibers by using a monocrystalline wafer; and after drying the collected fibers in a drying box, calcining the fibers at consistent temperature in a muffle furnace to obtain the bismuth ferrate nano fibers. The band gap of the bismuth ferrate nano fibers prepared by the preparation method is reduced from 3.2 to 3.4ev in the background technology to below 2.1ev.
Description
Technical field
The present invention relates to a kind of preparation method of nanofiber, particularly a kind of bismuth ferrate nano fiber preparation method.
Background technology
Photocatalyst material is exactly the chemical substance that under the exciting of photon, can play katalysis, is a kind of very important functional material.Photocatalysis technology is a kind of bionics techniques, is widely used in energy-conserving and environment-protective, new forms of energy, field, a plurality of forward position such as biological medicine.
Document " A.K.Alves, F.A.Berutti, F.J.Clemensb; T.Grauleb and C.P.Bergmann, Photocatalytic activity of titania fibers obtained by electrospinning, Materials ResearchBulletin; 2009,44,312-317 " discloses a kind of method for preparing photocatalysis material of titanium dioxide; This method adopts method of electrostatic spinning to prepare photocatalysis material of titanium dioxide, but the band gap width of this photocatalysis material of titanium dioxide is 3.2-3.4ev, because greater band gap; Can not well absorb visible light, can't satisfy requirement the sunshine efficient absorption.
Summary of the invention
In order to overcome the wide deficiency of existing photocatalyst material band gap, the present invention provides a kind of bismuth ferrate nano fiber preparation method.This method is dissolved into Hydrocerol A and forms citric acid solution in the deionized water; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent; Solution left standstill is placed on heated and stirred in the water-bath after placing; In solution, add Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, keep the concentration of Vinylpyrrolidone polymer; Utilize syringe pump and high-voltage power supply to carry out electrostatic spinning, collect fiber with monocrystalline silicon piece; The fiber of collecting placed put into retort furnace insulation calcining after the loft drier drying, obtain the bismuth ferrate nano fiber, this preparation method can reduce prepared bismuth ferrate nano fiber band gap width.
The technical solution adopted for the present invention to solve the technical problems: a kind of bismuth ferrate nano fiber preparation method is characterized in comprising the steps:
(a) Hydrocerol A is dissolved in the deionized water to form concentration be 0.2～0.4g/mL citric acid solution;
(b) with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein;
(c) solution left standstill of step (b) preparation is placed 24～72 hours after, be placed in the water-bath in 50～90 ℃ of heated and stirred 3～7 hours, in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.02～0.05g/mL;
(d) it is 1～3mm that the high polymeric solution that step (c) is prepared adds internal diameter to; Syringe needle is in the plastic injector of stainless steel syringe needle; Syringe is added in the syringe pump; Starting syringe pump, to make the injection flow velocity be 0.3～0.7mL/h, opens high-voltage power supply simultaneously and to syringe needle the voltage of 20～30kV is provided, and collects fiber with monocrystalline silicon piece;
(e) place loft drier to put into retort furnace after 4～8 hours the fiber of collecting and be warming up to 600～800 ℃, and, obtain the bismuth ferrate nano fiber in insulation calcining 4～8 hours with the heat-up rate of 1～5 ℃/min 100～150 ℃ of dryings.
The invention has the beneficial effects as follows: because this method is dissolved into Hydrocerol A and forms citric acid solution in the deionized water; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent; Solution left standstill is placed on heated and stirred in the water-bath after placing; In solution, add Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, keep the concentration of Vinylpyrrolidone polymer; Utilize syringe pump and high-voltage power supply to carry out electrostatic spinning, collect fiber with monocrystalline silicon piece; The fiber of collecting placed put into retort furnace insulation calcining after the loft drier drying, obtain the bismuth ferrate nano fiber, the prepared bismuth ferrate nano fiber band gap width of this preparation method is reduced to 2.0～2.1ev by 3.2～3.4ev of background technology.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Description of drawings
The ESEM collection of illustrative plates of Fig. 1 the inventive method embodiment 2 prepared bismuth ferrate nano fibers.
Fig. 2 the inventive method embodiment 2 prepared bismuth ferrate nano fibers visible light according under to the degradation rate curve of methyl orange solution.
Embodiment
Embodiment 1, earlier Hydrocerol A is dissolved into that to form concentration in the deionized water be the 0.2g/mL citric acid solution; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein; Solution left standstill is placed and to be placed it in after 48 hours in the water-bath in 60 ℃ of heated and stirred 4 hours, and in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.03g/mL; Adding this high polymeric solution to internal diameter at last is 2mm; Syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.3mL/h that the startup syringe pump makes the injection flow velocity; Open high-voltage power supply simultaneously and the voltage of 20kV is provided, collect fiber with monocrystalline silicon piece to syringe needle; Place loft drier to put into retort furnace after 8 hours 100 ℃ of dryings the fiber of collecting and be warming up to 650 ℃ with the heat-up rate of 3 ℃/min, insulation calcining 5 hours obtains the bismuth ferrate nano fiber.
Through detecting, the band gap width of the bismuth ferrate nano fiber of present embodiment preparation is 2.1ev.
Embodiment 2, earlier Hydrocerol A are dissolved into that to form concentration in the deionized water be the 0.4g/mL citric acid solution; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein; Solution left standstill is placed and to be placed it in after 24 hours in the water-bath in 50 ℃ of heated and stirred 7 hours, and in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.02g/mL; Adding this high polymeric solution to internal diameter at last is 1mm; Syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.7mL/h that the startup syringe pump makes the injection flow velocity; Open high-voltage power supply simultaneously and the voltage of 25kV is provided, collect fiber with monocrystalline silicon piece to syringe needle; Place loft drier to put into retort furnace after 5 hours 130 ℃ of dryings the fiber of collecting and be warming up to 750 ℃ with the heat-up rate of 1 ℃/min, insulation calcining 4 hours obtains the bismuth ferrate nano fiber.
Through detecting, the band gap width of the bismuth ferrate nano fiber of present embodiment preparation is 2.1ev.The fiber pattern that from the ESEM collection of illustrative plates of Fig. 1, can see preparation is good, and diameter is about 2 microns.The bismuth ferrate nano fiber that from Fig. 2, can see preparation has excellent more photochemical catalysis effect than the methyl orange solution that does not contain catalyzer.
Embodiment 3, earlier Hydrocerol A are dissolved into that to form concentration in the deionized water be the 0.3g/mL citric acid solution; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein; Solution left standstill is placed and to be placed it in after 72 hours in the water-bath in 70 ℃ of heated and stirred 6 hours, and in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.04g/mL; Adding this high polymeric solution to internal diameter at last is 3mm; Syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.4mL/h that the startup syringe pump makes the injection flow velocity; Open high-voltage power supply simultaneously and the voltage of 30kV is provided, collect fiber with monocrystalline silicon piece to syringe needle; Place loft drier to put into retort furnace after 4 hours 150 ℃ of dryings the fiber of collecting and be warming up to 800 ℃ with the heat-up rate of 5 ℃/min, insulation calcining 4 hours obtains the bismuth ferrate nano fiber.
Through detecting, the band gap width of the bismuth ferrate nano fiber of present embodiment preparation is 2.05ev.
Embodiment 4, earlier Hydrocerol A are dissolved into that to form concentration in the deionized water be the 0.3g/mL citric acid solution; Again with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein; Solution left standstill is placed and to be placed it in after 36 hours in the water-bath in 90 ℃ of heated and stirred 3 hours, and in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.05g/mL; Adding this high polymeric solution to internal diameter at last is 2mm; Syringe needle is in the plastic injector of stainless steel syringe needle, and syringe is added in the syringe pump, and it is 0.6mL/h that the startup syringe pump makes the injection flow velocity; Open high-voltage power supply simultaneously and the voltage of 25kV is provided, collect fiber with monocrystalline silicon piece to syringe needle; Place loft drier to put into retort furnace after 6 hours 140 ℃ of dryings the fiber of collecting and be warming up to 600 ℃ with the heat-up rate of 4 ℃/min, insulation calcining 8 hours obtains the bismuth ferrate nano fiber.
Through detecting, the band gap width of the bismuth ferrate nano fiber of present embodiment preparation is 2.0ev.
The present invention has also all done preparation to the technical scheme part parameter area of giving, and has all obtained good effect.
The bismuth ferrate nano fiber of the inventive method preparation has good microscopic appearance, under radiation of visible light, methyl orange solution is had good Degradation.Simultaneously preparation is simple for this bismuth ferrate nano fiber, so the method that the present invention prepares ferrous acid bismuth fiber is fit to industrialization promotion and scale operation, on the photochemical catalysis novel material, has broad application prospects.
Claims (1)
1. a bismuth ferrate nano fiber preparation method is characterized in that comprising the steps:
(a) Hydrocerol A is dissolved in the deionized water to form concentration be 0.2～0.4g/mL citric acid solution;
(b) with iron nitrate, Bismuth trinitrate add to stir to clarify in the citric acid solution transparent, the mol ratio 2: 1: 6 of iron nitrate, Bismuth trinitrate, Hydrocerol A wherein;
(c) solution left standstill of step (b) preparation is placed 24～72 hours after, be placed in the water-bath in 50～90 ℃ of heated and stirred 3～7 hours, in solution, adding molecular weight is 1.3 * 10
6Vinylpyrrolidone polymer, continue to be stirred to Vinylpyrrolidone polymer and dissolve fully, make the concentration of Vinylpyrrolidone polymer remain on 0.02～0.05g/mL;
(d) it is 1～3mm that the high polymeric solution that step (c) is prepared adds internal diameter to; Syringe needle is in the plastic injector of stainless steel syringe needle; Syringe is added in the syringe pump; Starting syringe pump, to make the injection flow velocity be 0.3～0.7mL/h, opens high-voltage power supply simultaneously and to syringe needle the voltage of 20～30kV is provided, and collects fiber with monocrystalline silicon piece;
(e) place loft drier to put into retort furnace after 4～8 hours the fiber of collecting and be warming up to 600～800 ℃, and, obtain the bismuth ferrate nano fiber in insulation calcining 4～8 hours with the heat-up rate of 1～5 ℃/min 100～150 ℃ of dryings.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011301A (en) * | 2012-12-28 | 2013-04-03 | 北京化工大学 | Erbium-doped bismuth ferrite multiferroic material and preparation method thereof |
| CN103074704A (en) * | 2013-01-22 | 2013-05-01 | 陕西科技大学 | Electrospinning preparation method of BiVO4 (bismuth vanadium oxide) fibers |
| CN103088457A (en) * | 2013-01-22 | 2013-05-08 | 陕西科技大学 | Method for preparing polyvinyl alcohol BiVO4 composite fiber by electrostatic spinning method |
| CN103193476A (en) * | 2013-05-03 | 2013-07-10 | 南京信息工程大学 | Wet chemical method for preparing pure phase BiFeO3 ceramics |
| CN104386757A (en) * | 2014-10-21 | 2015-03-04 | 天津师范大学 | One-dimensional bismuth ferrite nanotube as well as preparation method and application thereof |
| CN104549217A (en) * | 2013-10-11 | 2015-04-29 | 天津大学 | Photocatalyst bismuth vanadate nanofiber and preparation method and application thereof |
| CN105133090A (en) * | 2015-10-16 | 2015-12-09 | 河南泛锐复合材料研究院有限公司 | Preparation method for BiVO4 photocatalytic fiber material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659520A (en) * | 2009-09-17 | 2010-03-03 | 陕西科技大学 | Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method |
| CN101791558A (en) * | 2010-03-19 | 2010-08-04 | 上海师范大学 | Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof |
-
2011
- 2011-01-20 CN CN201110023191XA patent/CN102583566A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659520A (en) * | 2009-09-17 | 2010-03-03 | 陕西科技大学 | Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method |
| CN101791558A (en) * | 2010-03-19 | 2010-08-04 | 上海师范大学 | Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《Materials Letters》 20070816 Manoj Kumar et al. Large magnetization and weak polarization in sol-gel derived BiFeO3 ceramics 第1159-1161页 1 第62卷, * |
| MANOJ KUMAR ET AL.: "Large magnetization and weak polarization in sol–gel derived BiFeO3 ceramics", 《MATERIALS LETTERS》 * |
| S. H. XIE ET AL.: "Nanocrystalline multiferroic BiFeO3 ultrafine fibers by sol-gel based electrospinning", 《APPLIED PHYSICS LETTERS》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011301A (en) * | 2012-12-28 | 2013-04-03 | 北京化工大学 | Erbium-doped bismuth ferrite multiferroic material and preparation method thereof |
| CN103074704A (en) * | 2013-01-22 | 2013-05-01 | 陕西科技大学 | Electrospinning preparation method of BiVO4 (bismuth vanadium oxide) fibers |
| CN103088457A (en) * | 2013-01-22 | 2013-05-08 | 陕西科技大学 | Method for preparing polyvinyl alcohol BiVO4 composite fiber by electrostatic spinning method |
| CN103074704B (en) * | 2013-01-22 | 2015-01-28 | 陕西科技大学 | Electrospinning preparation method of BiVO4 (bismuth vanadium oxide) fibers |
| CN103088457B (en) * | 2013-01-22 | 2015-01-28 | 陕西科技大学 | Method for preparing polyvinyl alcohol BiVO4 composite fiber by electrostatic spinning method |
| CN103193476A (en) * | 2013-05-03 | 2013-07-10 | 南京信息工程大学 | Wet chemical method for preparing pure phase BiFeO3 ceramics |
| CN104549217A (en) * | 2013-10-11 | 2015-04-29 | 天津大学 | Photocatalyst bismuth vanadate nanofiber and preparation method and application thereof |
| CN104386757A (en) * | 2014-10-21 | 2015-03-04 | 天津师范大学 | One-dimensional bismuth ferrite nanotube as well as preparation method and application thereof |
| CN105133090A (en) * | 2015-10-16 | 2015-12-09 | 河南泛锐复合材料研究院有限公司 | Preparation method for BiVO4 photocatalytic fiber material |
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Application publication date: 20120718 |