CN110759385B - Bismuth ferrite nano cube material and preparation method and application thereof - Google Patents
Bismuth ferrite nano cube material and preparation method and application thereof Download PDFInfo
- Publication number
- CN110759385B CN110759385B CN201810824399.3A CN201810824399A CN110759385B CN 110759385 B CN110759385 B CN 110759385B CN 201810824399 A CN201810824399 A CN 201810824399A CN 110759385 B CN110759385 B CN 110759385B
- Authority
- CN
- China
- Prior art keywords
- bismuth ferrite
- bismuth
- ferrite nano
- solution
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 66
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 239000003513 alkali Substances 0.000 claims description 15
- 229910021645 metal ion Inorganic materials 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 11
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- 150000001621 bismuth Chemical class 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 239000002159 nanocrystal Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 17
- 239000002904 solvent Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 5
- 229910002897 Bi2Fe4O9 Inorganic materials 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- JANYNKCRWRNMFO-UHFFFAOYSA-N [Bi+3].[O-]Cl.[O-]Cl.[O-]Cl Chemical compound [Bi+3].[O-]Cl.[O-]Cl.[O-]Cl JANYNKCRWRNMFO-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000005303 antiferromagnetism Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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—
-
- B01J35/40—
-
- B01J35/50—
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
-
- 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 a bismuth ferrite nano cube material, and a preparation method and application thereof, and belongs to the technical field of nano material preparation, solar energy utilization and environmental protection. In particular to a wet chemical method, which adjusts the phase structure and the micro-morphology of bismuth ferrite by designing the reaction environment in the growth process of bismuth ferrite crystals. The invention successfully synthesizes the single-phase bismuth ferrite nano material with the rhombohedral phase structure under mild reaction conditions, solves the problem that impure phases are easy to generate when the bismuth ferrite material is prepared by adopting the traditional wet chemical synthesis method, and the prepared bismuth ferrite nano crystal has the size of 200nm-300nm, presents cubic morphology, can absorb sunlight in visible light wave bands, and can be used as a photocatalytic material to be applied to the purification of organic pollutants in the environment.
Description
Technical Field
The invention relates to the technical field of nano material preparation, solar energy utilization and environmental protection, in particular to a bismuth ferrite nano cubic material and a preparation method and application thereof.
Background
Bismuth ferrite is the only material with ferroelectric Curie temperature (T) and antiferromagnetic Neel transition temperature far higher than room temperatureC825 deg.C) and antiferromagnetic Neel temperature (T)N370 ℃), the material can realize the coexistence of room temperature ferroelectricity and antiferromagnetism, and simultaneously has strong magnetic/electric dipole coupling characteristics, and can realize the control of magnetization by electric field. The memory material has extremely important application prospect in the aspect of magnetic storage media, and can become a novel memory material integrating the advantages of ferroelectric materials and ferromagnetic materials, thereby being concerned. All in oneThen the residual polarization intensity (Pr) of the bismuth ferrite can reach 90-100 mu C/cm2The performance of lead zirconate titanate, a typical ferroelectric material used in practice, has been approached, which makes bismuth ferrite one of the important candidates for lead-free ferroelectrics. The research on bismuth ferrite has become a hot spot in the research field of multiferroic materials, and many scientists are attracted to the research field of the synthesis of a bismuth ferrite material system and the multiferroic physical mechanism thereof.
In addition, bismuth ferrite is due to Fe3+The energy gap of the rhombohedral phase single crystal, rhombohedral phase polycrystal and pseudo cubic perovskite structure is between 2.2eV and 2.7eV, the structure is mostly expressed as a direct band gap at room temperature, can effectively absorb visible light in solar spectrum, and is expected to be applied to the field of solar energy utilization as a photocatalytic material. However, the existing research shows that the temperature range of the synthesis and stable existence of the perovskite-structured bismuth ferrite material is narrow, the bismuth element in the component is more active and is easy to volatilize at high temperature and easy to hydrolyze in a liquid phase, so that the preparation process of the single-phase bismuth ferrite material is difficult to control, the process interval is narrow, and the synthesized product often contains Bi2Fe4O9、Bi25FeO40And the like, thereby affecting the performance and further going to the application. Therefore, the preparation method of the single-phase bismuth ferrite material with simple process and simple and convenient operation has important scientific significance and practical significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a single-phase bismuth ferrite multiferroic nano cubic material and application of the single-phase bismuth ferrite multiferroic nano cubic material in a photocatalytic material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a bismuth ferrite nano cubic material is a bismuth ferrite crystal with a single-phase diamond structure, the grain size is between 200 and 300nm, and the bismuth ferrite nano cubic material presents the cubic morphology.
The material has the forbidden band width of 2.2-2.5eV, and can absorb the light energy of ultraviolet and visible wave bands in the solar spectrum.
The preparation method of the bismuth ferrite nano cubic material comprises the following steps:
(1) preparing alkali liquor: fully dissolving alkali in the alcohol-water mixed solution to obtain alkali liquor, wherein the addition amount of the alkali in the alcohol-water mixed solution is 0.1-0.1075 g/mL; the alcohol-water mixed solution is a mixed solution of deionized water and absolute ethyl alcohol, wherein the volume ratio of water to absolute ethyl alcohol is 1:15-1: 10.
(2) Preparing a metal ion solution: adding bismuth chloride and ferric chloride into concentrated nitric acid to obtain a nitric acid solution of bismuth salt and ferric salt, namely the metal ion solution; wherein: the ratio of bismuth chloride to concentrated nitric acid was (0.2207-0.414) g: 1 mL; BiCl3With FeCl3The molar ratio of (A) to (B) is 1: 1; the concentrated nitric acid refers to commercial concentrated nitric acid, and the mass fraction is about 65-68%; the bismuth chloride and ferric chloride do not contain crystal water.
(3) Dropwise adding the metal ion solution obtained in the step (2) into the alkali liquor obtained in the step (1) under the condition of stirring, and stirring for 0.5-1h to obtain a reaction precursor solution; the volume ratio of the metal ion solution to the alkali liquor is 1:15-1: 16.
(4) Preserving the temperature of the reaction precursor solution obtained in the step (3) at the temperature of 180 ℃ and 200 ℃ for 6-12h, and naturally cooling to room temperature;
(5) and (4) repeatedly centrifuging and washing the precipitate obtained after cooling in the step (4), and drying in an oven at the temperature of 60 ℃ for 8-12 hours to obtain the bismuth ferrite nano cubic material.
The bismuth ferrite nano cubic material is directly applied to degradation of organic pollutants in the environment under sunlight irradiation.
The design idea of the invention is as follows:
the single-phase bismuth ferrite material is difficult to prepare, and the synthesized product containsWith Bi2Fe4O9、Bi25FeO40Adding a metal ion solution into an alkali liquor, stirring, and carrying out hydrothermal reaction on the obtained reaction precursor solution to synthesize the single-phase bismuth ferrite multiferroic material. In the preparation process, the polarity of the solvent and the solubility of the solute are changed by adjusting the proportion of deionized water and ethanol in the alkaline solvent, and single-phase bismuth ferrite is synthesized; the metal bismuth salt is easy to hydrolyze in deionized water to generate bismuth hypochlorite, so that the hydrolysis of the metal bismuth salt is inhibited by adding concentrated nitric acid; generally, the hydrothermal synthesis of bismuth ferrite needs to be carried out under strong alkaline conditions, so that NaOH is added to adjust the pH value of the bismuth ferrite.
The invention has the advantages that:
1. the invention synthesizes single-phase bismuth ferrite by adjusting the proportion of deionized water and ethanol in the alkali liquor and changing the polarity of the solvent and the solubility of the solute.
2. The invention utilizes the self-generated NaCl 'cage' to limit the growth of nano particles, and obtains the bismuth ferrite nano material with smaller size.
3. The invention has simple process flow, simple and convenient operation, low energy consumption and large output, and is suitable for mass production.
4. The bismuth ferrite synthesized by the method has the advantages of uniform size, regular appearance and special cubic morphology, does not use a surfactant, is beneficial to washing, and eliminates the possible adverse effect of the surfactant on the performance of the bismuth ferrite.
5. The bismuth ferrite has a small forbidden band width of about 2.2-2.5eV, can effectively absorb visible light, has a low valence band position, and has high photocatalytic oxidation activity.
Drawings
FIG. 1 is a structural representation of the prepared nano-scale bismuth ferrite crystal; wherein: (a) example 1 is a structural characterization, XRD pattern, of the prepared nano-scale bismuth ferrite crystal; (b) comparative example 1 is a structural characterization, XRD pattern, of the prepared nano-scale bismuth ferrite crystal.
FIG. 2 is an SEM image of the prepared nano-scale bismuth ferrite crystal.
FIG. 3 is a UV-VIS absorption curve of the nano-sized bismuth ferrite prepared in example 1.
FIG. 4 is a graph showing the relationship between the amount of methylene blue remaining at different treatment times and the time, when the nano-sized bismuth ferrite prepared in example 1 is excited by visible light.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
In the following examples, concentrated nitric acid was used at a concentration of 68 wt%, BiCl3、FeCl3Completely dissolving by stirring; BiCl3、FeCl3Do not contain crystal water to reduce the influence of crystal water on the solvent ratio.
Example 1
The preparation process of the single-phase bismuth ferrite multiferroic material of the embodiment is as follows:
(1) uniformly mixing 5mL of deionized water and 75mL of absolute ethyl alcohol, adding 8.6g of NaOH, and stirring for 1h to completely dissolve the NaOH to obtain an alkaline solvent;
(2) 1.1035g of BiCl were weighed out35ml of concentrated nitric acid was added thereto, and after stirring to completely dissolve bismuth chloride, 0.5675g of FeCl was added3After thorough stirring, BiCl is obtained3And FeCl3The metal ion solution of (4);
(3) dropwise adding the metal ion solution obtained in the step (2) into the alkali liquor obtained in the step (1) under the stirring condition, and stirring for 0.5h to obtain a precursor solution;
(4) transferring the precursor solution obtained in the step (3) into a reaction kettle with a polytetrafluoroethylene lining and a volume of 100mL, sealing, and then putting into an oven to store for 6h at 180 ℃;
(5) and cooling the reaction kettle to room temperature along with the furnace, repeatedly centrifuging the obtained precipitate, washing with water and ethanol, and drying in a 60 ℃ drying oven for 12 hours to obtain the nano bismuth ferrite material.
FIG. 1(a) is a xrd diagram of the bismuth ferrite nanomaterial prepared in this example, and it can be seen from FIG. 1(a) that the material is a single-phase bismuth ferrite crystal without any impurity phase.
Fig. 2 is an SEM image of the bismuth ferrite nanomaterial prepared in this embodiment, and it can be seen from fig. 2 that the prepared bismuth ferrite crystal has a uniform size and good dispersibility, and exhibits a cubic morphology.
Fig. 3 is a light absorption spectrum of the bismuth ferrite nanomaterial prepared in this embodiment, and it can be seen from fig. 3 that the bismuth ferrite nanomaterial exhibits a strong light absorption performance in the visible light absorption region. The absorption band edge is at the position of 570nm, and the band gap is about 2.2 eV.
Fig. 4 is a graph showing the relationship between the residual amount of methylene blue and time of the bismuth ferrite nanomaterial prepared in this embodiment under the excitation of visible light, and it can be seen from fig. 4 that the bismuth ferrite nanomaterial has a good degradation effect on methylene blue.
Example 2
The preparation process of the single-phase bismuth ferrite multiferroic material of the embodiment is as follows:
(1) uniformly mixing 5mL of deionized water and 75mL of absolute ethyl alcohol, adding 8.6g of NaOH, and stirring for 1h to completely dissolve the NaOH to obtain an alkaline solvent;
(2) 2.207g of BiCl were weighed out35ml of concentrated nitric acid was added thereto, and after stirring to completely dissolve bismuth chloride, 1.135g of FeCl was added3After thorough stirring, BiCl is obtained3And FeCl3The metal ion solution of (4);
(3) dropwise adding the metal ion solution obtained in the step (2) into the alkali liquor obtained in the step (1) under the stirring condition, and stirring for 0.5h to obtain a suspension;
(4) transferring the precursor solution obtained in the step (3) into a reaction kettle with a polytetrafluoroethylene lining and a volume of 100mL, sealing, and then putting into an oven to store for 6h at 180 ℃;
(5) and cooling the reaction kettle to room temperature along with the furnace, repeatedly centrifuging the obtained precipitate, washing with water and ethanol, and drying in a 60 ℃ drying oven for 12 hours to obtain the nano bismuth ferrite material.
Comparative example 1
The preparation process of the single-phase bismuth ferrite multiferroic material of the embodiment is as follows:
(1) uniformly mixing 2mL of deionized water and 78mL of absolute ethyl alcohol, adding 8.6g of NaOH, and stirring for 1h to completely dissolve the NaOH to obtain an alkaline solvent;
(2) 2.207g of BiCl were weighed out3To which is added5ml of concentrated nitric acid was added, stirred to completely dissolve bismuth chloride, and 1.135g of FeCl was added3After thorough stirring, BiCl is obtained3And FeCl3The metal ion solution of (4);
(3) dropwise adding the metal ion solution obtained in the step (2) into the alkali liquor obtained in the step (1) under the stirring condition, and stirring for 0.5h to obtain a precursor solution;
(4) transferring the precursor solution obtained in the step (3) into a reaction kettle with a polytetrafluoroethylene lining and a volume of 100mL, sealing, and then putting into an oven to store for 6h at 180 ℃;
(5) and cooling the reaction kettle to room temperature along with the furnace, repeatedly centrifuging the obtained precipitate, washing with water and ethanol, and drying in a 60 ℃ drying oven for 12 hours to obtain the nano bismuth ferrite material.
FIG. 1(b) is a xrd diagram of the bismuth ferrite nano-material prepared by the present example, and it can be seen from FIG. 1(b) that BiFeO exists in the material except for3In addition to Bi and Bi2Fe4O9Peak of iso-phase.
Claims (3)
1. A preparation method of a bismuth ferrite nano cubic material is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) preparing alkali liquor: fully dissolving NaOH in the alcohol-water mixed solution to obtain an alkali solution, wherein the addition amount of the NaOH in the alcohol-water mixed solution is 0.1-0.1075 g/mL; the alcohol-water mixed solution is a mixed solution of deionized water and absolute ethyl alcohol, wherein the volume ratio of water to absolute ethyl alcohol is 1:15-1: 10;
(2) preparing a metal ion solution: adding bismuth chloride and ferric chloride into concentrated nitric acid to obtain a nitric acid solution of bismuth salt and ferric salt, namely the metal ion solution; wherein: the ratio of bismuth chloride to concentrated nitric acid was (0.2207-0.414) g: 1 mL; BiCl3With FeCl3The molar ratio of (A) to (B) is 1: 1;
(3) dropwise adding the metal ion solution obtained in the step (2) into the alkali liquor obtained in the step (1) under the condition of stirring, and stirring for 0.5-1h to obtain a reaction precursor solution; the volume ratio of the metal ion solution to the alkali liquor is 1:15-1: 16;
(4) transferring the reaction precursor solution obtained in the step (3) to a reaction kettle, sealing, and then carrying out hydrothermal reaction, wherein the hydrothermal reaction is carried out at 180-200 ℃ for 6-12h, and then naturally cooling to room temperature;
(5) repeatedly centrifuging and washing the precipitate obtained after cooling in the step (4), and drying in an oven at 60 ℃ for 8-12 hours to obtain the bismuth ferrite nano cubic material;
the prepared bismuth ferrite nano cubic material is a single-phase diamond-phase bismuth ferrite crystal, the grain size is between 200 and 300nm, and the cubic shape is presented;
the forbidden band width of the bismuth ferrite nano cubic block material is 2.2-2.5eV, and the bismuth ferrite nano cubic block material can absorb light energy of ultraviolet and visible wave bands in solar spectrum.
2. The method for preparing bismuth ferrite nano-cubic material according to claim 1, characterized in that: in the step (2), the mass fraction of the concentrated nitric acid is 65-68%.
3. The method for preparing bismuth ferrite nano-cubic material according to claim 1, characterized in that: in the step (2), the bismuth chloride and the ferric chloride do not contain crystal water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810824399.3A CN110759385B (en) | 2018-07-25 | 2018-07-25 | Bismuth ferrite nano cube material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810824399.3A CN110759385B (en) | 2018-07-25 | 2018-07-25 | Bismuth ferrite nano cube material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110759385A CN110759385A (en) | 2020-02-07 |
| CN110759385B true CN110759385B (en) | 2021-10-15 |
Family
ID=69327015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810824399.3A Active CN110759385B (en) | 2018-07-25 | 2018-07-25 | Bismuth ferrite nano cube material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110759385B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811472B (en) * | 2021-01-11 | 2022-11-18 | 重庆工商大学 | Calcium ferrite gas sensing material, preparation method and application |
| CN113336271B (en) * | 2021-06-11 | 2022-06-28 | 浙江理工大学 | Micron-sized regular square strip Bi2Fe4O9Preparation method, product and application of multiferroic material |
| CN113336272B (en) * | 2021-06-11 | 2022-04-08 | 浙江理工大学 | Hollow square strip-shaped single-phase Bi2Fe4O9Preparation method, product and application of multiferroic material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850621A (en) * | 2006-05-26 | 2006-10-25 | 上海大学 | Method for preparing bismuth oxide nano powder |
| WO2012094110A2 (en) * | 2011-01-07 | 2012-07-12 | Baker Hughes Incorporated | Filtration of dangerous or undesirable contaminants |
| CN105329870A (en) * | 2015-12-14 | 2016-02-17 | 长沙理工大学 | Preparing method for Rubik-cube-shaped sillenite bismuth phosphate powder |
| CN107626321A (en) * | 2017-10-08 | 2018-01-26 | 南京邮电大学 | One kind quickly prepares different morphologies BiFeO3The method of photochemical catalyst |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009115506A2 (en) * | 2008-03-19 | 2009-09-24 | Basf Se | Metallic nanoparticles stabilised with derivatisied polyethylenimines or polyvinylamines |
-
2018
- 2018-07-25 CN CN201810824399.3A patent/CN110759385B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850621A (en) * | 2006-05-26 | 2006-10-25 | 上海大学 | Method for preparing bismuth oxide nano powder |
| WO2012094110A2 (en) * | 2011-01-07 | 2012-07-12 | Baker Hughes Incorporated | Filtration of dangerous or undesirable contaminants |
| CN105329870A (en) * | 2015-12-14 | 2016-02-17 | 长沙理工大学 | Preparing method for Rubik-cube-shaped sillenite bismuth phosphate powder |
| CN107626321A (en) * | 2017-10-08 | 2018-01-26 | 南京邮电大学 | One kind quickly prepares different morphologies BiFeO3The method of photochemical catalyst |
Non-Patent Citations (2)
| Title |
|---|
| Controlled Fabrication of BiFeO3 Uniform Microcrystals and Their Magnetic and Photocatalytic Behaviors;Shun Li et al.;《JOURNAL OF PHYSICAL CHEMISTRY C》;20100402;第114卷;第2903-2908页和附图1、3、6 * |
| Shun Li et al..Controlled Fabrication of BiFeO3 Uniform Microcrystals and Their Magnetic and Photocatalytic Behaviors.《JOURNAL OF PHYSICAL CHEMISTRY C》.2010,第114卷第2903-2908页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110759385A (en) | 2020-02-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110759385B (en) | Bismuth ferrite nano cube material and preparation method and application thereof | |
| CN101890354B (en) | Method for preparing bismuth ferrite photocatalyst | |
| CN102925979B (en) | Method for preparing perovskite lead titanate crystal nanosheet | |
| Wang et al. | Chemical co-precipitation synthesis and properties of pure-phase BiFeO3 | |
| CN103894177B (en) | A kind of synthetic method with the rear-earth-doped metatitanic acid potassium powder of photocatalytic activity | |
| CN103242042B (en) | Method for preparing multibasic oxide nanometer particles based on core-shell structure three-dimensional micro-solid-phase reaction. | |
| CN108689422B (en) | Preparation method of large-specific-surface-area nano gadolinium oxide powder | |
| CN109665537A (en) | A kind of low temperature preparation EuB6The method of nanocube crystal | |
| CN109205655B (en) | Preparation method of nano gadolinium oxide with particle size of 80-100nm | |
| CN103570068B (en) | A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof | |
| CN104528799A (en) | Preparation method of ultrafine magnesium-based rare earth hexaaluminate powder | |
| CN103896335A (en) | Preparation method of nano-porous titanium dioxide with high specific surface | |
| CN104150539A (en) | Preparation method of YFeO3 nanopowder | |
| CN103922405B (en) | A kind of mass synthetic method of even mg-doped lithium niobate polycrystal | |
| CN107662948B (en) | Preparation method of tungsten trioxide nanosheet | |
| CN103566925B (en) | A kind of preparation method of rear-earth-doped mesoporous pucherite | |
| CN101591176A (en) | A kind of synthetic Gd 3Ga 5O 12(GGG) the nanocrystalline method of crystalline ceramics | |
| CN104445341A (en) | Preparation method of pure YAG (Yttrium Aluminum Garnet) phase type yttrium aluminum garnet nanometer powder | |
| CN103449511A (en) | Strontium titanate submicron crystal and preparation method thereof | |
| CN108640158B (en) | Preparation method of high-purity hexagonal sheet barium ferrite | |
| CN104001493A (en) | Preparation method of octahedral PbTiO3-TiO2 composite nanometer photocatalyst | |
| KR20150088409A (en) | Method of forming a gdc/lscf composite powder | |
| Wang et al. | Facile preparation, characterization and photocatalytic properties of multifunctional BiFeO3 nanocrystals | |
| CN113336271B (en) | Micron-sized regular square strip Bi2Fe4O9Preparation method, product and application of multiferroic material | |
| Jing et al. | Magnetic Core–Shell Nano-TiO2/Al2O3/NiFe2O4 Microparticles with Enhanced Photocatalytic Activity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |