CN104195642B - One prepares monocrystalline BiFeO3the method of nanometer sheet - Google Patents
One prepares monocrystalline BiFeO3the method of nanometer sheet Download PDFInfo
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- CN104195642B CN104195642B CN201410412805.7A CN201410412805A CN104195642B CN 104195642 B CN104195642 B CN 104195642B CN 201410412805 A CN201410412805 A CN 201410412805A CN 104195642 B CN104195642 B CN 104195642B
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Abstract
The invention discloses one and prepare monocrystalline BiFeO3The method of nanometer sheet, comprises the following steps: by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in salpeter solution and is made into female saline solution；CTAB is dissolved in organic solvent, prepares two groups of CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, stirs to obtain solution A；KOH solution is added drop-wise in another group CTAB solution, stirs to obtain solution B；Solution B is added drop-wise in solution A, after stirring, obtains hydro-thermal reaction predecessor；Hydro-thermal reaction predecessor, solvent are put in water heating kettle；Seal water heating kettle, in 140～160 DEG C of baking ovens, react 12～24h, filter to obtain precipitate；Precipitate is scrubbed, dried monocrystalline BiFeO3Nanometer sheet.The present invention can synthesize pure phase monocrystal BiFeO at low temperatures3Nanometer sheet, saves the energy, and product degree of crystallinity is high, and technique is easily controlled, and equipment needed thereby is simple.
Description
Technical field
The present invention relates to BiFeO3The preparation method of nano-powder, prepares monocrystalline BiFeO particularly to one3The method of nanometer sheet.
Background technology
Multi-ferroic material has ferroelectricity, ferromagnetism or ferroelasticity due to it simultaneously, and has a wide range of applications at aspects such as information recording device, spin electric device and sensors.In numerous multi-ferroic materials, BiFeO3Relatively especially, it is one of a few single-phase multi-ferroic material being at room temperature provided simultaneously with ferroelectric order and antiferromagnetic order of having now been found that, and its Curie temperature and Neel temperature are higher, respectively 1103K and 643K, thus are studied the most widely.Additionally, due to its energy gap the narrowest (～2.1eV), there is in visible-range good photoresponse, the hugest in the using value of photocatalysis field.But, the leakage current that caused due to the existence of dephasign is excessive seriously hampers BiFeO3The application of material.
BiFeO so far3Synthetic method have a lot, mainly have high temperature solid-phase sintering method and polymer precursor method, the chemical method such as sol-gel process and coprecipitation.High temperature solid-state method repeatability is the best, and needs after the sintering to wash away Bi with nitric acid2Fe4O9And Bi25FeO40Deng dephasign, the powder surface making synthesis is coarse.And using the chemical methods such as polymer precursor method, coprecipitation, sol-gel process, microemulsion method such as to still need to sinter at a temperature of higher than 400 DEG C, energy consumption is higher, and particle diameter skewness and morphology microstructure can be caused irregular, finally affects the performance of material.
The catalytic capability of photocatalyst is relevant with its purity, specific surface area, crystallization degree etc..Purity the highest (without dephasign), crystallization degree is the highest, and specific surface area is the biggest, and the catalytic capability of photocatalyst is the strongest.Nanometer sheet, owing to having big specific surface area, is provided that more reaction active site, and can improve the quantum efficiency that interface charge shifts, so the photocatalyst with nano-sheet pattern has higher catalysis activity.So far both at home and abroad about preparing monocrystalline BiFeO3The report of nanometer sheet is few.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide one and prepare monocrystalline BiFeO3The method of nanometer sheet, can synthesize pure phase monocrystal BiFeO at 140 DEG C～160 DEG C3Nanometer sheet, saves the energy, and monocrystalline BiFeO3Nanometer sheet degree of crystallinity is high, and technique is easily controlled, and the required instrument and equipment of synthesis is simple.
The purpose of the present invention is achieved through the following technical solutions:
One prepares monocrystalline BiFeO3The method of nanometer sheet, comprises the following steps:
(1) 1:1 weighs analytically pure Fe (NO in molar ratio3)3·9H2O and Bi (NO3)3·5H2O, and be dissolved in mass concentration be 8～10% salpeter solution in, be made into uniform female saline solution by magnetic agitation；The concentration of described female saline solution is 0.05～0.15mol/L；
(2) weigh CTAB, and be dissolved in organic solvent, prepare the CTAB solution that two groups of concentration is 0.1～0.25mol/L；
(3) being added drop-wise to by mother's saline solution in one group of CTAB solution, obtain solution A through magnetic agitation, female saline solution is 1:5～1:2 with the ratio of the volume of CTAB solution；By being added drop-wise in another group CTAB solution with female the 10 of saline solution same volume～the KOH solution of 30mol/L, obtaining solution B through magnetic agitation, KOH solution is 1:5～1:2 with the ratio of the volume of CTAB solution；
(4) solution B is added drop-wise in solution A, and after magnetic agitation, is precipitated thing, prepare hydro-thermal reaction predecessor；
(5) being put in water heating kettle hydro-thermal reaction predecessor prepared by step (4), and add solvent, making water heating kettle compactedness is 70%～80%；
(6) seal water heating kettle, water heating kettle is placed in 140 DEG C～160 DEG C of baking ovens, take out the product in water heating kettle after reaction 12～24h, be precipitated thing through filtering；Precipitate is scrubbed, obtains monocrystalline BiFeO after drying3Nanometer sheet.
Step (2) described organic solvent is the mixed solution of hexamethylene and n-butyl alcohol.
In the mixed solution of described hexamethylene and n-butyl alcohol, the volume ratio of hexamethylene and n-butyl alcohol is 3:1～6:1.
Step (4) is described to be added drop-wise to solution B in solution A, particularly as follows:
Solution B is added drop-wise in solution A with the rate of titration less than 5mL/min.
Described dry temperature is 80 DEG C.
Step (5) described solvent is hexamethylene.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) BiFeO prepared by the present invention3Powder body is monocrystalline BiFeO3Nanometer sheet, complete crystallization, crystalline phase is single.Due to monocrystalline BiFeO3Nanometer sheet has the characteristic that specific surface area is big, can be as the photocatalyst of degradation of contaminant under visible ray, further, it is also possible to be used for making information recording device of good performance, spin electric device and sensor.
(2) present invention prepare monocrystalline BiFeO3The method of nanometer sheet, preparation temperature is 140 DEG C～160 DEG C, and the chemical method such as existing solid sintering technology and polymer precursor method, sol-gel process and coprecipitation is compared, and temperature is greatly lowered, and saves the energy.
(3) present invention prepare monocrystalline BiFeO3The method of nanometer sheet, product need not process through follow-up sintering, and technology controlling and process and the required instrument and equipment of synthesis are simple, reduce further production cost.
(4) present invention prepare monocrystalline BiFeO3The method of nanometer sheet, the reactant precursor solution prepared need not be filtered, washed and dried, and further shorten technique manufacturing cycle.
(5) present invention prepare monocrystalline BiFeO3The method of nanometer sheet, raw material configures in the liquid phase, the uniform mixing that the content of each component is accurately controlled and realizes on molecule/atomic level, the monocrystalline BiFeO of preparation3Nanometer sheet has the advantages such as purity height and good dispersion.
Accompanying drawing explanation
Fig. 1 is the monocrystalline BiFeO prepared by embodiments of the invention 13The preparation flow figure of nanometer sheet.
Fig. 2 is the monocrystalline BiFeO prepared by embodiments of the invention 13The x-ray diffraction collection of illustrative plates of nanometer sheet
Fig. 3 is the monocrystalline BiFeO prepared by embodiments of the invention 13The transmission electron microscope photo of nanometer sheet.
Fig. 4 is the monocrystalline BiFeO prepared by embodiments of the invention 13The high-resolution-ration transmission electric-lens photo of nanometer sheet.
Fig. 5 is the monocrystalline BiFeO prepared by embodiments of the invention 13The transmission electron microscope SEAD style of nanometer sheet.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
As it is shown in figure 1, the BiFeO of the present embodiment3Nanometer sheet preparation process comprises the following steps:
Weigh 1mmol analytically pure Fe (NO3)3·9H2O and 1mmol Bi (NO3)3·5H2O, and be dissolved in the salpeter solution that mass concentration is 8% of 10ml, by magnetic agitation 0.5h, it is made into uniform female saline solution；Preparing two groups of identical CTAB solution of concentration, often the process for preparation of group CTAB solution is as follows: weighs 1gCTAB, and is dissolved in the mixed solution of 20ml hexamethylene and 4ml n-butyl alcohol, by magnetic agitation 0.5h, obtains CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, and magnetic agitation 0.5h obtains solution A；The KOH solution of the 10mol/L of 10ml is added drop-wise in another group CTAB solution, and magnetic agitation 0.5h obtains solution B；Again solution B is added drop-wise in solution A with the rate of titration of 4.5mL/min, and magnetic agitation 0.5h prepares hydro-thermal reaction predecessor；Being put in water heating kettle by above-mentioned hydro-thermal reaction predecessor, and add hexamethylene, making compactedness is 80%.Seal water heating kettle, water heating kettle is placed in 140 DEG C of baking ovens, after reaction 16h, take out the product in water heating kettle, through filtering to obtain precipitate more scrubbed, drying to obtain monocrystalline BiFeO in the baking oven of 80 DEG C3Nanometer sheet.
Fig. 2 is BiFeO prepared by the present embodiment3The x-ray diffraction collection of illustrative plates of nano-powder, as shown in Figure 2, pure phase BiFeO prepared by the present embodiment3Nano-powder degree of crystallinity is high.
Fig. 3 is BiFeO prepared by the present embodiment3The transmission electron microscope picture of nano-powder, from the figure 3, it may be seen that BiFeO prepared by the present embodiment3Powder body is rectangular nanometer sheet, and its marginal dimension is (70～130) nm × (90～200) nm.
Fig. 4 is the BiFeO prepared by embodiments of the invention 13The high-resolution-ration transmission electric-lens photo of nanometer sheet, as it can be seen, its interplanar distance is 0.39nm, corresponding to BiFeO3(012) crystal face.
Fig. 5 is the BiFeO prepared by embodiments of the invention 13The transmission electron microscope SEAD style of nanometer sheet, as seen from the figure, BiFeO3Nanometer sheet is monocrystalline.
Embodiment 2
Weigh 1mmol analytically pure Fe (NO3)3·9H2O and 1mmol Bi (NO3)3·5H2O, and be dissolved in the salpeter solution of 9% of 8ml, by magnetic agitation 0.5h, it is made into uniform female saline solution；Preparing two groups of identical CTAB solution of concentration, often the process for preparation of group CTAB solution is as follows: weighs 1.5gCTAB, and is dissolved in the mixed solution of 20ml hexamethylene and 4ml n-butyl alcohol, by magnetic agitation 0.5h, obtains CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, and magnetic agitation 0.5h obtains solution A；The KOH solution of the 10mol/L of 8ml is added drop-wise in another group CTAB solution, and magnetic agitation 0.5h obtains solution B；Again solution B is added drop-wise in solution A with the rate of titration of 4mL/min, and magnetic agitation 0.5h prepares hydro-thermal reaction predecessor；Being put in water heating kettle by above-mentioned hydro-thermal reaction predecessor, and add hexamethylene, making compactedness is 70%.Seal water heating kettle, water heating kettle is placed in 140 DEG C of baking ovens, after reaction 12h, takes out the product in water heating kettle, through filtering to obtain precipitate, the most scrubbed, in the baking oven of 80 DEG C, its marginal dimension of drying to obtain is the monocrystalline BiFeO of (80～130) nm × (80～200) nm3Nanometer sheet.
Embodiment 3
Weigh 1mmol analytically pure Fe (NO3)3·9H2O and 1mmol Bi (NO3)3·5H2O, and be dissolved in the salpeter solution of 9% of 10ml, by magnetic agitation 0.5h, it is made into uniform female saline solution；Preparing two groups of identical CTAB solution of concentration, often the process for preparation of group CTAB solution is as follows: weighs 2gCTAB, and is dissolved in the mixed solution of 24ml hexamethylene and 4ml n-butyl alcohol, by magnetic agitation 0.5h, obtains CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, and magnetic agitation 0.5h obtains solution A；The KOH solution of the 10mol/L of 10ml is added drop-wise in another group CTAB solution, and magnetic agitation 0.5h obtains solution B；Again solution B is added drop-wise in solution A with the rate of titration of 4mL/min, and magnetic agitation 0.5h prepares hydro-thermal reaction predecessor；Being put in water heating kettle by above-mentioned hydro-thermal reaction predecessor, and add hexamethylene, making compactedness is 80%.Seal water heating kettle, water heating kettle is placed in 160 DEG C of baking ovens, after reaction 24h, takes out the product in water heating kettle, through filtering to obtain precipitate, the most scrubbed, in the baking oven of 80 DEG C, drying to obtain marginal dimension is the monocrystalline BiFeO of (60～120) nm × (80～160) nm3Nanometer sheet.
Embodiment 4
Weigh 1mmol analytically pure Fe (NO3)3·9H2O and 1mmol Bi (NO3)3·5H2O, and be dissolved in the salpeter solution of 10% of 8ml, by magnetic agitation 0.5h, it is made into uniform female saline solution；Preparing two groups of identical CTAB solution of concentration, often the process for preparation of group CTAB solution is as follows: weighs 1.5gCTAB, and is dissolved in the mixed solution of 22.5ml hexamethylene and 4.5ml n-butyl alcohol, by magnetic agitation 0.5h, obtains CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, and magnetic agitation 0.5h obtains solution A；The KOH solution of the 20mol/L of 8ml is added drop-wise in another group CTAB solution, and magnetic agitation 0.5h obtains solution B；Again solution B is added drop-wise in solution A with the rate of titration of 4.5mL/min, and magnetic agitation 0.5h prepares hydro-thermal reaction predecessor；Being put in water heating kettle by above-mentioned hydro-thermal reaction predecessor, and add hexamethylene, making compactedness is 75%.Seal water heating kettle, water heating kettle is placed in 140 DEG C of baking ovens, after reaction 16h, takes out the product in water heating kettle, through filtering to obtain precipitate, the most scrubbed, in the baking oven of 80 DEG C, its marginal dimension of drying to obtain is the monocrystalline BiFeO of (80～140) nm × (80～180) nm3Nanometer sheet.
Embodiment 5
Weigh 1mmol analytically pure Fe (NO3)3·9H2O and 1mmol Bi (NO3)3·5H2O, and be dissolved in the salpeter solution of 10% of 8ml, by magnetic agitation 0.5h, it is made into uniform female saline solution；Preparing two groups of identical CTAB solution of concentration, often the process for preparation of group CTAB solution is as follows: weighs 1gCTAB, and is dissolved in the mixed solution of 20ml hexamethylene and 4ml n-butyl alcohol, by magnetic agitation 0.5h, obtains CTAB solution；Mother's saline solution is added drop-wise in one group of CTAB solution, and magnetic agitation 0.5h obtains solution A；The KOH solution of the 30mol/L of 8ml is added drop-wise in another group CTAB solution, and magnetic agitation 0.5h obtains solution B；Again solution B is added drop-wise in solution A with the rate of titration of 4.5mL/min, and magnetic agitation 0.5h prepares hydro-thermal reaction predecessor；Being put in water heating kettle by above-mentioned hydro-thermal reaction predecessor, and add hexamethylene, making compactedness is 70%.Seal water heating kettle, water heating kettle is placed in 150 DEG C of baking ovens, after reaction 16h, takes out the product in water heating kettle, through filtering to obtain precipitate, the most scrubbed, in the baking oven of 80 DEG C, its marginal dimension of drying to obtain is the monocrystalline BiFeO of (70～120) nm × (80～190) nm3Nanometer sheet.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted by the embodiments; the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1. prepare monocrystalline BiFeO for one kind3The method of nanometer sheet, it is characterised in that comprise the following steps:
(1) 1:1 weighs analytically pure Fe (NO in molar ratio3)3·9H2O and Bi (NO3)3·5H2O, and by it
Be dissolved in mass concentration be 8～10% salpeter solution in, be made into uniform female saline solution by magnetic agitation；
The concentration of described female saline solution is 0.05～0.15mol/L；
(2) weighing CTAB, and be dissolved in organic solvent, preparing two groups of concentration is 0.1～0.25mol/L
CTAB solution；
(3) mother's saline solution is added drop-wise in one group of CTAB solution, obtains solution A, female salt through magnetic agitation
Solution is 1:5～1:2 with the ratio of the volume of CTAB solution；By 10～30mol/L with female saline solution same volume
KOH solution be added drop-wise to another group CTAB solution in, obtain solution B, KOH solution through magnetic agitation
It is 1:5～1:2 with the ratio of the volume of CTAB solution；
(4) solution B is added drop-wise in solution A, and after magnetic agitation, is precipitated thing, prepare hydro-thermal anti-
Answer predecessor；
(5) hydro-thermal reaction predecessor prepared by step (4) is put in water heating kettle, and add solvent hexamethylene
Alkane, making water heating kettle compactedness is 70%～80%；
(6) seal water heating kettle, water heating kettle is placed in 140 DEG C～160 DEG C of baking ovens, takes out after reaction 12～24h
Product in water heating kettle, is precipitated thing through filtering；Precipitate is scrubbed, obtains monocrystalline BiFeO after drying3
Nanometer sheet.
The most according to claim 1 prepare monocrystalline BiFeO3The method of nanometer sheet, it is characterised in that step
Suddenly (2) described organic solvent is the mixed solution of hexamethylene and n-butyl alcohol.
The most according to claim 2 prepare monocrystalline BiFeO3The method of nanometer sheet, it is characterised in that institute
Stating in the mixed solution of hexamethylene and n-butyl alcohol, the volume ratio of hexamethylene and n-butyl alcohol is 3:1～6:1.
The most according to claim 1 prepare monocrystalline BiFeO3The method of nanometer sheet, it is characterised in that step
Suddenly (4) are described is added drop-wise to solution B in solution A, particularly as follows:
Solution B is added drop-wise in solution A with the rate of titration less than 5mL/min.
The most according to claim 1 prepare monocrystalline BiFeO3The method of nanometer sheet, it is characterised in that institute
Stating dry temperature is 80 DEG C.
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| CN106140177A (en) * | 2015-03-16 | 2016-11-23 | 中智环保新材料江苏有限公司 | A kind of superstructure visible light responsive BiFeO3the preparation method and application of photocatalyst |
| CN105129861B (en) * | 2015-08-27 | 2017-04-12 | 华南理工大学 | Preparation method for bismuth ferrite BiFeO3 nanosheet |
| CN109626440B (en) * | 2019-01-17 | 2021-06-25 | 天津城建大学 | BiFeO preparation based on hydrothermal method3Method for nanosheet and BiFeO3Nano-sheet |
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