CN104211125A - Immobilized nano porous BiFeO3 and preparation method thereof - Google Patents
Immobilized nano porous BiFeO3 and preparation method thereof Download PDFInfo
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- CN104211125A CN104211125A CN201410450770.6A CN201410450770A CN104211125A CN 104211125 A CN104211125 A CN 104211125A CN 201410450770 A CN201410450770 A CN 201410450770A CN 104211125 A CN104211125 A CN 104211125A
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Abstract
The invention discloses an immobilized nano porous BiFeO3 material and a preparation method thereof. The method comprises the following steps: firstly preparing a NiO/macroscopic base material monolithic catalyst by virtue of a dipping method, heating to 550 DEG C to 600 DEG C under nitrogen protection and then feeding CH4, C2H4 or CO under a normal pressure so as to grow carbon nanofibers; then feeding N2 to blow away the rest of CH4, C2H4 or CO, cooling to a room temperature, dipping the obtained carbon nanofibers solidified on a macroscopic base material into an ethanol solution of a metal nitrate containing Bi and Fe, carrying out suction filtration, sequentially drying an obtained sample at 120 DEG C and 300 DEG C for 0.5 hour each time, repeatedly carrying out dipping and suction filtration and drying for 3 to 4 times; and finally, roasting the sample in the air by controlling the temperature within 475 DEG C to 525 DEG C so as to obtain the immobilized nano porous BiFeO3 material with a good orientation. The immobilized nano porous BiFeO3 material is simple in preparation process, controllable in shape, low in production cost and high in repeatability.
Description
Technical field
The present invention relates to a kind of immobilization nanoporous BiFeO
3and preparation method thereof, belong to field of inorganic materials.
Background technology
Bismuth ferrite (BiFeO
3) as a kind of ferroelectric material and piezoelectric, because it has the advantage of fatigue resistance and high-curie temperature, have in microwave, storage, sensor and smart machine etc. and well apply potential.Meanwhile, BiFeO
3with the electronic structure of its uniqueness, excellent visible absorption ability and higher organic matter degradation ability, cause the great interest of the numerous investigators of photocatalysis field.
The BiFeO reported at present
3preparation method have multiple, mainly contain high temperature solid phase synthesis, sol-gel method, hydrothermal method, coprecipitation method, combustion method etc.Utilize the BiFeO that aforesaid method prepares
3sample mainly exists with nanometer powder state, and powder catalyst in use can exist a lot of unfavorable drawback, such as Pressure Drop and heat trnasfer problem and contact efficiency is low is difficult to be separated with catalyzer and is easy to loss etc.Therefore, a kind of immobilization BiFeO is developed
3technology of preparing, then more and more receive the concern of numerous investigators to obtaining a large amount of, favorable orientation, pattern and structure-controllable sample.
Carbon nano fiber is as a kind of novel carbon material, chemical vapor deposition (CVD) method that can be simple by technique, with low cost prepares, it is as a kind of emerging mould material in recent years, has very wide application prospect in field of composite material preparation.Carbon nano fiber mould plate technique is adopted to utilize pickling process can realize nanoporous BiFeO
3be solidificated on macroscopical body material, and by optimal preparation technology condition, finally can obtain the type material of high-quality macroscopical matrix and microscopic particles phase compound, such material is expected to show more excellent catalytic performance in the application of visible light photocatalytic degradation organic dye, and this mainly comes from BiFeO
3be solidificated on macroscopical body material and can well solve powder photocatalyst material unfavorable drawback existing in actual use, thus there is potential actual application prospect, have not yet to see the report about this respect work.
Summary of the invention
An object of the present invention is to provide a kind of immobilization nanoporous BiFeO
3material.
Two of object of the present invention is to provide above-mentioned a kind of immobilization nanoporous BiFeO
3the preparation method of material.
Technical scheme of the present invention
A kind of immobilization nanoporous BiFeO
3material, is prepared by a method comprising the following steps and forms:
(1), synthesis of nano carbon fiber on macroscopical body material;
1. pickling process, is adopted to prepare NiO/ macroscopic view body material integer catalyzer
Macroscopical body material is immersed in the Ni (NO that concentration is 0.3mol/L
3)
26H
210min in the ethanolic soln of O, then carries out vacuum filtration, 110 DEG C of dryings, to remove the superfluous Ni (NO of macroscopical substrate material surface
3)
2.6H
2o ethanolic soln, puts into the flat-temperature zone of crystal reaction tube after drying, control temperature be 300 DEG C carry out roasting after obtain NiO/ macroscopic view body material integer catalyzer;
Described macroscopical body material is SiO
2rod-like fibre, honeycomb ceramic body or porous anodic alumina films; The present invention is in a preferred embodiment only with macroscopical matrix SiO of ordered structure
2rod-like fibre is illustrated, but the macroscopical body material such as honeycomb ceramic body or the porous anodic alumina films etc. that do not limit ordered structure are preparing the nanoporous BiVO with orderly macrostructure
4in application;
2., chemical Vapor deposition process is adopted to prepare carbon nano fiber on macroscopical body material
Step 1. roasting pass into nitrogen protection after obtaining NiO/ macroscopic view body material integer catalyzer thereupon and by temperature program, the temperature of crystal reaction tube risen to 550-600 DEG C by 300 DEG C simultaneously, then pass into the CH that flow is 200-400mL/min under normal pressure
4, C
2h
4or the carbonaceous gas 2-3h such as CO, to carry out the growth of carbon nano fiber, then pass into the N of 15-30min
2to blow away the CH of surplus
4, C
2h
4or the carbonaceous gas such as CO, finally crystal reaction tube is cooled to room temperature, the carbon nano fiber on macroscopical body material must be solidificated in;
(2), to be solidificated in carbon nano fiber on macroscopical body material for templated synthesis BiFeO
3;
By the carbon nano fiber be solidificated on macroscopical body material of the 2. gained in step (1), the total concn be immersed in containing Bi and Fe is 5-15min in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L; then suction filtration is in order to remove the ethanolic soln of the metal nitrate containing Bi and Fe of surface excess, and the sample of gained is successively through 120 DEG C of drying treatment 0.5h, 300 DEG C of drying treatment 0.5h;
The described total concn containing Bi and Fe is in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, and the mol ratio of Bi and Fe is 1:1;
Repeat above-mentioned dipping, suction filtration and drying treatment operation 3-4 time, finally control temperature is carry out roasting at 475-525 DEG C to remove carbon nano fiber template in atmosphere, finally obtains the nanoporous BiFeO be solidificated on macroscopical body material
3material and immobilization nanoporous BiFeO
3material;
The described total concn containing Bi and Fe is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, by Bi(NO
3)
36H
2o joins in the ethanolic soln containing concentrated nitric acid, adds Fe(NO after stirring under magnetic stirring apparatus
3)
39H
2o continues to be uniformly mixed, and the total concn namely obtaining metal Bi and Fe is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L;
The described ethanolic soln containing concentrated nitric acid, the volume ratio of concentrated nitric acid and ethanol is 1:14-20; Adding appropriate concentrated nitric acid in ethanol is to suppress Bi
3+hydrolysis.
beneficial effect of the present invention
A kind of immobilization nanoporous BiFeO of the present invention
3material, is a kind of macroscopical body material and the functional materials of microcosmic particle phase compound, adopts carbon nano fiber template to utilize pickling process by BiFeO
3be solidificated on dissimilar macroscopical body material, and effectively can regulate and control the formation of carbon nano fiber template by the condition controlling chemical vapour deposition, and then effectively regulate and control BiFeO
3formation, therefore a kind of immobilization nanoporous BiFeO of the present invention
3have a large amount of, favorable orientation, the advantages such as morphology controllable, can towards application-specific.
A kind of immobilization nanoporous BiFeO of the present invention
3it is a kind of macroscopical body material and the functional materials of microcosmic particle phase compound, the various drawbacks using Conventional nano fine catalyst to bring can be replaced, such as Pressure Drop and heat trnasfer problem and contact efficiency is low is difficult to be separated with catalyzer, thus there is potential application prospect.
A kind of immobilization nanoporous BiFeO of the present invention
3first the preparation method of material, namely adopt chemical Vapor deposition process (CVD) synthesis of nano carbon fiber template, is then that template utilizes pickling process by BiFeO with carbon nano fiber
3on material cured macroscopic view body material, then carbon nano fiber is removed in roasting, finally the obtained BiFeO be solidificated on macroscopical body material
3, therefore, its preparation technology is simple, low production cost and repeatability is high, effectively can be regulated and controled the formation of carbon nano fiber template, and then regulate and control a kind of immobilization nanoporous BiFeO by the condition controlling chemical vapour deposition
3formation.
Accompanying drawing explanation
Fig. 1, be solidificated in SiO
2carbon nano fiber on fiber amplifies the scanning electron microscope sem figure of 5000 times;
Fig. 2, be solidificated in SiO
2carbon nano fiber on fiber amplifies the scanning electron microscope sem figure of 40000 times;
Fig. 3, be solidificated in SiO
2nanoporous BiFeO on fiber
3amplify the scanning electron microscope sem figure of 5000 times;
Fig. 4, be solidificated in SiO
2nanoporous BiFeO on fiber
3amplify the scanning electron microscope sem figure of 20000 times;
Fig. 5, be solidificated in SiO
2nanoporous BiFeO on fiber
3the XRD figure of X-ray powder diffraction;
Fig. 6, be solidificated in SiO
2nanoporous BiFeO on fiber
3uV-Visible diffuse spectrogram.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
embodiment 1
A kind of immobilization nanoporous BiFeO
3material, is prepared by a method comprising the following steps and forms:
(1), at macroscopical body material SiO
2synthesis of nano carbon fiber on rod-like fibre;
1. pickling process, is adopted to prepare NiO/ macroscopic view body material SiO
2rod-like fibre integer catalyzer
By macroscopical body material SiO of 0.2g
2rod-like fibre is immersed in the Ni (NO that concentration is 0.3mol/L
3)
2.6H
2in the ethanolic soln of O, then vacuum filtration, 110 DEG C of macroscopical body material SiO of dry removal
2ni (the NO of rod-like fibre surface excess
3)
2.6H
2o solution, then put into long for the 100cm diameter flat-temperature zone control temperature that is the crystal reaction tube of 6cm be 300 DEG C carry out roasting after obtain the macroscopical body material SiO of NiO/
2rod-like fibre integer catalyzer;
The NiO/ macroscopic view body material SiO of above-mentioned gained
2rod-like fibre integer catalyzer, calculates in mass ratio, i.e. NiO: macroscopical body material SiO
2rod-like fibre is 5:100;
2., chemical Vapor deposition process is adopted to prepare carbon nano fiber template
Step 1. roasting obtain NiO/ macroscopic view body material SiO
2rod-like fibre integer catalyzer passes into nitrogen protection thereupon, and by temperature control program, the temperature of crystal reaction tube is risen to 550 DEG C of protection 1h by 300 DEG C simultaneously, then passes into the carbonaceous gas CH that flow is 320mL/min under condition of normal pressure
4, control reaction times 2h to carry out the growth of carbon nano fiber, after having reacted, pass into 15min N again
2in order to blow away surplus carbonaceous gas CH
4, finally crystal reaction tube is cooled to room temperature, macroscopical body material SiO must be solidificated in
2carbon nano fiber on rod-like fibre;
Above-mentioned gained be solidificated in macroscopical body material SiO
2carbon nano fiber on rod-like fibre amplifies the scanning electron microscope sem figure of 5000,40000 times respectively as shown in Figure 1 and Figure 2, as can be seen from Figure 1 carbon nano fiber evenly and a large amount of load at macroscopical body material SiO
2on rod-like fibre, and weave in forms the carbon nano fiber layer of dense regular mutually, and the diameter of carbon nano fiber is about 60-80nm as can be seen from Figure 2;
In addition, SiO
2rod-like fibre diameter is about 9.7 μm, further by the SEM figure contrast before and after chemical vapour deposition, can calculate at macroscopical body material SiO
2about 2.4 μm of the carbon nano fiber thickness that rod-like fibre generates;
(2), nanoporous BiFeO
3at macroscopical body material SiO
2solidification on rod-like fibre body material
1., containing the preparation of the ethanolic soln of the metal nitrate of Bi and Fe
By 2.43g(0.005mol) Bi(NO
3)
35H
2the bismuth source of O joins in the ethanolic soln of the concentrated nitric acid of 50mL, stirs, add 2.02g(0.005mol under magnetic stirring apparatus) Fe(NO
3)
39H
2the source of iron of O, continues to be stirred to and mixes, and obtains the ethanolic soln of the metal nitrate of total concn 0.2 mol/L containing Bi and Fe;
In the ethanolic soln of described concentrated nitric acid, the volume ratio of concentrated nitric acid and ethanol is 1:14-20;
What 2., step (1) obtained is solidificated in macroscopical body material SiO
2carbon nano fiber on rod-like fibre is immersed in 10min in the ethanolic soln of the metal nitrate of the above-mentioned total concn 0.2mol/L containing Bi and Fe, then vacuum filtration is in order to remove the ethanolic soln of its surface excess containing the metal nitrate of Bi and Fe, and the filter cake of gained is successively through 120 DEG C of dry 0.5h and 300 DEG C dry 0.5h;
Repeat above-mentioned dipping, suction filtration and drying process 3 times;
Last in atmosphere at 500 DEG C roasting 5h to remove carbon nano fiber template, thus obtain being solidificated in macroscopical body material SiO
2nanoporous BiFeO on rod-like fibre body material
3, i.e. immobilization nanoporous BiFeO
3material.
Above-mentioned gained be solidificated in macroscopical body material SiO
2nanoporous BiFeO on rod-like fibre body material
3the scanning electron microscope sem figure amplifying 5000,20000 times as shown in Figure 3, Figure 4, can find out nanoporous BiFeO from Fig. 3, Fig. 4
3a large amount of and uniform coating load is at macroscopical body material SiO
2on rod-like fibre, thus form the BiFeO of dense regular
3layer, can also calculate at macroscopical body material SiO from Fig. 3,4
2the nanoporous BiFeO that rod-like fibre generates
3about 2.9 μm of thick coating.And find from powerful scanning electron microscopic observation, prepared nanoporous BiFeO
3coating is that fibrous porous structural load is at macroscopical body material SiO
2on rod-like fibre, thus replicate pattern when carbon nano fiber template is not removed.
Above-mentioned gained be solidificated in macroscopical body material SiO
2nanoporous BiFeO on rod-like fibre body material
3i.e. immobilization nanoporous BiFeO
3as shown in Figure 5, what as can be seen from Figure 5 adopt carbon nano fiber template to utilize pickling process to prepare is solidificated in macroscopical body material SiO for the X-ray powder diffraction figure of material and XRD figure
2nanoporous BiFeO on rod-like fibre body material
3i.e. immobilization nanoporous BiFeO
3biFeO is mainly in the XRD figure of material sample
3characteristic diffraction peak, just has micro-dephasign peak to exist, and this shows that the present invention adopts carbon nano fiber template to utilize pickling process can prepare the higher BiFeO of purity
3.
Above-mentioned gained be solidificated in macroscopical body material SiO
2nanoporous BiFeO on rod-like fibre body material
3i.e. immobilization nanoporous BiFeO
3as shown in Figure 6, what as can be seen from Figure 6 adopt carbon nano fiber template to utilize pickling process to prepare is solidificated in macroscopical body material SiO for the UV-Vis reflective spectrum of material and UV-Via
2nanoporous BiFeO on rod-like fibre body material
3i.e. immobilization nanoporous BiFeO
3material sample has very wide photoresponse scope in visible region, and has good visible absorption ability, and therefore such material is expected to show more excellent catalytic performance in visible light catalytic reaction, and this mainly comes from BiFeO
3be solidificated on macroscopical body material and can well solve powder photocatalyst material unfavorable drawback existing in actual use, thus there is potential actual application prospect.
In sum, carbon nano fiber template is adopted to utilize pickling process can by nanoporous BiFeO
3be solidificated on macroscopical body material.Carbon nano fiber template can realize nanoporous BiFeO
3be solidificated on dissimilar macroscopical body material, and effectively can regulate and control the formation of carbon nano fiber template by the condition controlling chemical vapour deposition, and then effectively regulate and control nanoporous BiFeO
3formation, finally can obtain high quality macroscopic view matrix and the nanoporous BiFeO of microscopic particles compound
3material.
Above said content be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (6)
1. an immobilization nanoporous BiFeO
3material, is characterized in that described immobilization nanoporous BiFeO
3material is prepared by a method comprising the following steps and forms:
(1), synthesis of nano carbon fiber on macroscopical body material;
1. pickling process, is adopted to prepare NiO/ macroscopic view body material integer catalyzer
Macroscopical body material is immersed in the Ni (NO that concentration is 0.3mol/L
3)
26H
25-15min in the ethanolic soln of O, then carries out vacuum filtration, 110 DEG C of dryings, puts into the flat-temperature zone of crystal reaction tube after drying, control temperature be 300 DEG C carry out roasting after obtain NiO/ macroscopic view body material integer catalyzer;
Described macroscopical body material is SiO
2rod-like fibre, honeycomb ceramic body or porous anodic alumina films;
2., chemical Vapor deposition process is adopted to prepare carbon nano fiber on macroscopical body material
Step 1. roasting pass into nitrogen protection after obtaining NiO/ macroscopic view body material integer catalyzer thereupon and by temperature program, the temperature of crystal reaction tube risen to 550-600 DEG C by 300 DEG C simultaneously; then the carbonaceous gas 2-3h that flow is 200-400mL/min is passed under normal pressure; to carry out the growth of carbon nano fiber, then pass into the N of 15-30min
2, finally crystal reaction tube is cooled to room temperature, the carbon nano fiber on macroscopical body material must be solidificated in;
Described carbonaceous gas is CH
4, C
2h
4or CO;
(2), to be solidificated in carbon nano fiber on macroscopical body material for templated synthesis BiFeO
3;
By the carbon nano fiber be solidificated on macroscopical body material of the 2. gained in step (1), the total concn be immersed in containing Bi and Fe is 5-15min in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, and then suction filtration, gained sample are successively through 120 DEG C of drying treatment 0.5h, 300 DEG C of drying treatment 0.5h;
Repeat above-mentioned dipping, suction filtration and drying treatment operation 3-4 time, finally control temperature is carry out roasting at 475-525 DEG C, being finally fixed nanoporous BiFeO in atmosphere
3material;
The described total concn containing Bi and Fe is in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, and the mol ratio of Bi and Fe is 1:1.
2. a kind of immobilization nanoporous BiFeO as claimed in claim 1
3material, is characterized in that the total concn containing Bi and Fe described in step (2) of its preparation process is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, by Bi(NO
3)
36H
2o joins in the ethanolic soln containing concentrated nitric acid, adds Fe(NO after stirring under magnetic stirring apparatus
3)
39H
2o continues to be uniformly mixed, and the total concn namely obtaining metal Bi and Fe is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L;
The described ethanolic soln containing concentrated nitric acid, the volume ratio of concentrated nitric acid and ethanol is 1:14-20.
3. a kind of immobilization nanoporous BiFeO as claimed in claim 1
3material, is characterized in that the total concn containing Bi and Fe described in step (2) of its preparation process is the ethanolic soln of the metal nitrate of 0.2mol/L.
4. a kind of immobilization nanoporous BiFeO as claimed in claim 1
3the preparation method of material, is characterized in that specifically comprising the steps:
(1), synthesis of nano carbon fiber on macroscopical body material;
1. pickling process, is adopted to prepare NiO/ macroscopic view body material integer catalyzer
Macroscopical body material is immersed in the Ni (NO that concentration is 0.3mol/L
3)
26H
25-15min in the ethanolic soln of O, then carries out vacuum filtration, 110 DEG C of dryings, puts into the flat-temperature zone of crystal reaction tube after drying, control temperature be 300 DEG C carry out roasting after obtain NiO/ macroscopic view body material integer catalyzer;
Described macroscopical body material is SiO
2rod-like fibre, honeycomb ceramic body or porous anodic alumina films;
2., chemical Vapor deposition process is adopted to prepare carbon nano fiber on macroscopical body material
Step 1. roasting pass into nitrogen protection after obtaining NiO/ macroscopic view body material integer catalyzer thereupon and by temperature program, the temperature of crystal reaction tube risen to 550-600 DEG C by 300 DEG C simultaneously; then the carbonaceous gas 2-3h that flow is 200-400mL/min is passed under normal pressure; to carry out the growth of carbon nano fiber, then pass into the N of 15-30min
2, finally crystal reaction tube is cooled to room temperature, the carbon nano fiber on macroscopical body material must be solidificated in;
Described carbonaceous gas is CH
4, C
2h
4or CO;
(2), to be solidificated in carbon nano fiber on macroscopical body material for templated synthesis BiFeO
3;
By the carbon nano fiber be solidificated on macroscopical body material of the 2. gained in step (1), the total concn be immersed in containing Bi and Fe is 5-15min in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, and then suction filtration, gained sample are successively through 120 DEG C of drying treatment 0.5h, 300 DEG C of drying treatment 0.5h;
Repeat above-mentioned dipping, suction filtration and drying treatment operation 3-4 time, finally control temperature is carry out roasting at 475-525 DEG C, being finally fixed nanoporous BiFeO in atmosphere
3material;
The described total concn containing Bi and Fe is in the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, and the mol ratio of Bi and Fe is 1:1.
5. a kind of immobilization nanoporous BiFeO as claimed in claim 4
3the preparation method of material, is characterized in that the total concn containing Bi and Fe described in step (2) is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L, by Bi(NO
3)
36H
2o joins in the ethanolic soln containing concentrated nitric acid, adds Fe(NO after stirring under magnetic stirring apparatus
3)
39H
2o continues to be uniformly mixed, and the total concn namely obtaining metal Bi and Fe is the ethanolic soln of the metal nitrate of 0.05-0.2mol/L;
The described ethanolic soln containing concentrated nitric acid, the volume ratio of concentrated nitric acid and ethanol is 1:14-20.
6. a kind of immobilization nanoporous BiFeO as claimed in claim 4
3the preparation method of material, is characterized in that the total concn containing Bi and Fe described in step (2) is the ethanolic soln of the metal nitrate of 0.2mol/L.
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| CN110935421A (en) * | 2019-12-17 | 2020-03-31 | 扬州大学 | Method for adsorption treatment of hexavalent chromium-containing wastewater by bismuth ferrite modified charcoal compound |
| CN111774062A (en) * | 2020-06-04 | 2020-10-16 | 东南大学 | BiFeO3Preparation method of particle-carbon fiber composite catalyst |
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| CN110935421A (en) * | 2019-12-17 | 2020-03-31 | 扬州大学 | Method for adsorption treatment of hexavalent chromium-containing wastewater by bismuth ferrite modified charcoal compound |
| CN111774062A (en) * | 2020-06-04 | 2020-10-16 | 东南大学 | BiFeO3Preparation method of particle-carbon fiber composite catalyst |
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Application publication date: 20141217 |