CN106698521A - Three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof - Google Patents
Three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses three-dimensional flower-shaped bismuth ferrite powder and a preparation method thereof. The preparation method comprises the following steps: taking Bi(nO3)3.5H2O and Fe(NO3)3.9H2O as starting materials, preparing blocky bismuth ferrite powder by adopting a hydrothermal method, then mixing the bismuth ferrite powder, a corrosive solvent, a reducing agent and a complex agent under the protective atmosphere, and obtaining three-dimensional porous bismuth ferrite flower balls by adopting a one-step corrosion method. According to the invention, a thick flaky Bi2Fe4O9 powder raw material is prepared by adopting the hydrothermal method, grains are uniform in size and shape and are better in dispersibility, a corrosion technology is adopted, preparation technological operation is simple, and the period is short; and the prepared flower-shaped bismuth ferrite has the diameter being about 1-2mu m, sizes are uniform, a specific surface area is relatively large due to a porous structure, and performances of all the aspects are respectively improved.
Description
【Technical field】
The invention belongs to material science, and in particular to a kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof.
【Background technology】
Bismuth iron series compound is a huge family, including sillenite type and Ca-Ti ore type, due to its physical property
It is of considerable interest with technological applications.In recent years, it has been found that the Ca-Ti ore type bismuth iron compound of unsymmetric structure has
This phenomenon that the property that ferroelectricity and magnetic coexist, ferroelectricity and magnetic coexist, that is, many iron effects not only have an opportunity to grind
Study carefully the physics on basis.Bi2Fe4O9Structurally ordered with two kinds, it is found to be a kind of good manufacture Semiconductor gas sensors sensing
The material of device, and it or a kind of catalyst.Bi2Fe4O9It is low-gap semiconductor, applying can have in photocatalysis field
The absorption of effect and the visible luminous energy of utilization, and be conducive to reclaiming with weak ferromagnetism.It effectively can be carried out using visible ray
Light-catalysed generation catalyst, has application prospect at aspects such as using energy source, wastewater treatment, purification of air.Additionally, porous material
Application in catalysis and separation and also obtain people as optics and nano-reactor and more and more pay close attention to, Er Qie
The numerous areas such as chemistry, photoelectronics, electromagnetism, materialogy, environmentology have huge potential using value.
Bi is prepared at present2Fe4O9The most common method of powder mainly has sol-gel process, molten-salt growth method, solid phase method and hydro-thermal
Method.YangZ. closelypacked Bi is successfully prepared using citrate Sol-Gel technology combined aluminum oxide template2Fe4O9Receive
Rice noodles.Et al. ZhangM. Bi is successfully prepared using polyacrylamide gel method2Fe4O9Powder.Zhang X. et al. utilize water
Thermal synthesis technology, successfully obtains the crystal of the submicron-scale of favorable dispersibility.By adjusting mineralising agent concentration, can obtain
Obtain the crystal of laminar, tabular and cube bulk；Under the conditions of KOH concentration (12M) high, addition polyvinyl alcohol is lived as surface
Property agent, can obtain bar-shaped and fibrous Bi2Fe4O9Crystal.
And the Bi of the single shape such as nano particle, nano square, nano wire and sub-micrometer rod2Fe4O9Specific surface area it is most
Smaller, very many performances are limited.
【The content of the invention】
It is an object of the invention to provide a kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof, corroded by a step
Method, prepares the three-dimensional flower-shaped bismuth ferrite powder with high specific surface area.
For achieving the above object, the present invention is adopted the following technical scheme that：
Comprise the following steps：
Step 1：The bismuth ferrite powder of slab-like and corrosion solvent are pressed into (2.5~3) mg：1mL mixes, and carries out ultrasound point
Dissipate, obtain mixed liquor A；
Step 2：Under protective atmosphere, mixed liquor A is carried out into heating water bath and is stirred, while to body is added dropwise in mixed liquor A
Product is than being (2~4)：1 reducing agent and complexing agent, carry out corrosion reaction, wherein, the volume ratio of corrosion solvent and reducing agent is (80
~100)：4；Cooled down rapidly after 40~50min of reaction, terminating reaction；
Step 3：The sediment obtained after step 2 is reacted is washed and dried, and obtains three-dimensional flower-shaped ferrous acid bismuth meal
Body.
Further, the preparation process of the bismuth ferrite powder of slab-like includes in step 1：
A () takes Bi (NO respectively3)3·5H2O、Fe(NO3)3·9H2O, water and nitric acid, magnetic agitation after mixing make its abundant
Dissolving obtains mixed liquid B；Wherein, Bi (NO3)3·5H2O、Fe(NO3)3·9H2The ratio of O, water and nitric acid is 1mmol：2mmol：
(10~15) mL：(1~2) mL；
B () after obtaining suspension C russet, continues to stir to NaOH solution is slowly added dropwise in mixed liquid B；
C suspension C is poured into reactor and sealed by (), carry out homogeneous hydro-thermal reaction, generates sediment；
D () question response kettle is cooled to room temperature after, the sediment washing that homogeneous hydro-thermal reaction is obtained obtains sheet after drying
The bismuth ferrite powder of shape.
Further, the mass fraction of nitric acid is 65% in step (a)；In step (b) concentration of NaOH solution be 10~
12mol/L, drop rate is per second two drops.
Further, the condition of homogeneous hydro-thermal reaction is in step (c)：Reaction temperature is in 180~200 DEG C, reaction time
In 6~12h.
Further, in step (d), the sediment that homogeneous hydro-thermal reaction is obtained is washed by deionized water and absolute ethyl alcohol
Wash, 8~12h is then dried at 60~80 DEG C.
Further, in step 1, corrosion solvent is DMF；Reducing agent is hydrazine hydrate, complexing in step 2
Agent is methyl thioglycolate.
Further, in step 1,20~30min of ultrasonic disperse.
Further, in step 2, protective atmosphere is nitrogen or inert gas；Water bath heating temperature is 70~80 DEG C.
Further, rapid cooling is carried out using -2~2 DEG C of supercooling absolute ethyl alcohol in step 2 to terminate；Corrosion reaction is obtained
To sediment absolute ethyl alcohol and deionized water wash respectively until pH in neutrality, then at 60~80 DEG C dry 6~
12h。
Bismuth ferrite powder of the present invention is three-dimensional flower-shaped sphere structure of the diameter that is self-assembly of of nanometer sheet at 1~2 μm.
Compared with prior art, the device have the advantages that：The present invention is prepared for slab-like by hydro-thermal method first
Bi2Fe4O9Powder, then carries out corrosion process by a step etch, and three-dimensional flower-shaped Bi is obtained2Fe4O9Powder, increases
Big Bi2Fe4O9Specific surface area, corrosion before and after Bi2Fe4O9Specific surface area be respectively 0.84m2/ g and 41.04m2/ g, lifting
Nearly 50 times.Hydro-thermal method is used out to prepare out raw material sheet Bi in the present invention2Fe4O9Powder, is conducive to Bi2Fe4O9Crystal grain is big
Small shape is uniform and dispersiveness is preferable.The present invention uses etching process, and the grain dispersion after corrosion is uniform, and used by preparation
Condition can be controlled preferably.The present invention obtains three-dimensional flower ball-shaped Bi2Fe4O9Method it is novel, particle is uniform and equipment is grasped
It is required that low, process is simple, energy consumption are low, can operate continuously and process condition is easily controlled.
Obtained three-dimensional flower-shaped Bi of the invention2Fe4O9Powder purity is high, crystallinity is good, pattern is uniform, and what is obtained is
A kind of flower-like structure that nanometer sheet is self-assembly of, diameter is about 1~2 μm, and compared to the slab-like bismuth ferrite before corrosion, it compares table
Area is larger, tests prove that, it can be degradable in 3 hours to methyl orange sample under ultraviolet light, and before adding corrosion
The sample of bismuth ferrite is only degraded 20%.
【Brief description of the drawings】
Fig. 1 is Bi prepared by hydro-thermal method of the present invention2Fe4O9The XRD of powder.
Fig. 2 is the three-dimensional flower-shaped Bi that the present invention is prepared2Fe4O9XRD.
Fig. 3 is Bi prepared by hydro-thermal method of the present invention2Fe4O9The SEM figures of powder.
Fig. 4 is the three-dimensional flower-shaped Bi that the present invention is prepared2Fe4O9SEM figure.
【Specific embodiment】
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
A kind of three-dimensional flower-shaped Bi2Fe4O9And preparation method thereof, comprise the following steps：
1) according to Bi2Fe4O9In mol ratio weigh mol ratio respectively for 1mmol：Bi (the NO of 2mmol3)3·5H2O,
Fe(NO3)3·9H2O, measures 10~15mL water and 1~2mL concentrated nitric acids (65wt.%), magnetic agitation after mixing, makes it fully molten
Solution obtains mixed liquor A；The nitrate for adding concentrated nitric acid purpose to be bismuth and iron can be completely dissolved in the aqueous solution, make bismuth from
The amount of son and iron ion carries out ensuing reaction in whole solution with original proportioning.
2) to the NaOH solution for being added dropwise over 45~50mL, 10~12mol/L in mixed liquor A with the speed of per second two drops,
With precipitate B i3+And Fe3+, after obtaining suspension B russet, continue to stir；NaOH concentration in the scope of 10~12mol/L,
The sheet bismuth ferrite that purity is higher and is evenly distributed can be obtained.
3) suspension B is poured into ptfe autoclave, is placed in homogeneous reactor and seals, carry out homogeneous hydro-thermal anti-
Should, the reaction condition of homogeneous reaction：At 180~200 DEG C, the reaction time is controlled in 6~12h for reaction temperature control；
4) after question response kettle is cooled to room temperature, the precipitation that will be obtained after reaction passes through deionized water and absolute ethanol washing
Afterwards, 8~12h is dried in the vacuum drying chamber at 60~80 DEG C, bismuth ferrite powder is obtained.
5) by step 4) in the bismuth ferrite powder that obtains and DMF be mixed in silk mouthful bottle, ultrasonic disperse
20~30min；Bismuth ferrite powder and N, the mass volume ratio of N-dimethylformamide is 2.5~3mg：1mL.
6) silk mouthful bottle is carried out heating water bath and is stirred, water bath heating temperature is 70~80 DEG C, while be passed through nitrogen continuing
Protection；
7) it is 2~4 to volume ratio is added dropwise in mixed liquor:1 hydrazine hydrate and methyl thioglycolate, nitrogen is persistently protected
Shield, after reaction carries out 40~50min, adds -2~2 DEG C of the rapid terminating reaction of cold ethanol；N in corrosion process, N dimethyl first
The volume ratio of acid amides and hydrazine hydrate is 80~100:4.
8) sediment that will be obtained after reaction dries 6 after absolute ethyl alcohol and deionized water are washed at 60~80 DEG C
~12h, obtains the bismuth ferrite powder of loose structure.
Nitrogen, or the such as inert gas such as helium, neon or argon gas can be used in the present invention as protective atmosphere, row
Except the oxygen in reaction solution, it is to avoid methyl thioglycolate oxidation deactivation, wherein nitrogen low cost, and liquid nitrogen storage to get up more pacify
Entirely.Therefore preferably it is passed through nitrogen sustainable protection in corrosion process.
The present invention is with Bi (NO3)3·5H2O and Fe (NO3)3·9H2O is initiation material, and the iron of slab-like is prepared with hydro-thermal method
Sour bismuth meal body, then with DMF as solvent, hydrazine hydrate is reducing agent, methyl thioglycolate is complexing agent, through a step
Etch, by the addition of hydrazine hydrate, ferric ion is reduced into ferrous iron, due to solvent DMF and network
The collective effect of mixture methyl thioglycolate, nanometer sheet is peeled off into by the bismuth ferrite of slab-like, and final these nanometer sheets are by certainly
Assembling forms micron-sized flower-shaped spheroid, obtains the bismuth ferrite bouquet of three-dimensional porous structure.Preparation technology of the present invention is simple to operate,
Cycle is short；The flower-shaped bismuth ferrite diameter prepared is about 1~2 μm, and uniform in size, compared to the slab-like bismuth ferrite before corrosion, it compares
Surface area is larger, and correlated performance also increases.
Embodiment 1
A kind of three-dimensional flower-shaped Bi2Fe4O9And preparation method thereof, comprise the following steps：
(1) according to Bi2Fe4O9In mol ratio weigh respectively mole be 1mmol Bi (NO3)3·5H2O, 2mmol
Fe (NO3)3·9H2O, 10mL water and 1mL concentrated nitric acids (65wt.%), magnetic agitation after mixing, make it fully dissolve and are mixed
Close liquid A；
(2) to being slowly added dropwise 45mL 10mol/L NaOH solutions in mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B is poured into ptfe autoclave, carries out homogeneous hydro-thermal reaction, reaction temperature is 180 DEG C,
Time is 6h；
(4) after question response kettle is cooled to room temperature, the precipitation that will be obtained after reaction passes through deionized water and absolute ethanol washing
Afterwards, it is put into 60 DEG C of baking oven and dries 12h, obtains bismuth ferrite powder；
(5) DMF of bismuth ferrite powder 3mg and 1mL is mixed in silk mouthful bottle, ultrasonic disperse 20min；
(6) heating water bath at silk mouthful bottle being placed in into 80 DEG C, and start stirring, it is passed through nitrogen；
(7) it is 4 to ratio is added dropwise in mixed liquor:1 hydrazine hydrate and methyl thioglycolate, nitrogen sustainable protection, instead
After 45min should being carried out, 0 DEG C of the rapid terminating reaction of cold ethanol is added；N in corrosion process, N-dimethylformamide：Hydrazine hydrate
Volume ratio is 90:4.
(8) sediment that will be obtained after reaction is put into 60 DEG C of dryings of baking oven after absolute ethyl alcohol and deionized water are washed
6h, obtains the bismuth ferrite powder of loose structure.
Fig. 1 and Fig. 2 are respectively the XRD of the front and rear bismuth ferrite of corrosion under the reaction condition, it can be seen that prepared by hydro-thermal method
Bi2Fe4O9Without dephasign generation, crystallinity is preferable, the Bi after step corrosion process treatment2Fe4O9Still generated without dephasign.And it is rotten
Bi after erosion2Fe4O9Substantially reduced before diffraction peak intensity is relatively corrosive.Corrosion is front and rear under Fig. 3 and Fig. 4 are respectively the reaction condition
The SEM figures of bismuth ferrite, the Bi that as can be seen from the figure hydro-thermal method is prepared2Fe4O9Crystal grain is 1 μm~1.5 μm or so of the length of side, thick
The slab-like of degree 200nm or so, surface is smooth and smooth, and shape is uniform, favorable dispersibility；By after step corrosion process treatment
The Bi for obtaining2Fe4O9It is about 1 μm~2 μm of three-dimensional flower-shaped spheroid for diameter, from surface it can be seen that being nanometer sheet self assembly shape
Into flower-like structure, it is uniform in size.
Embodiment 2
The reaction time of corrosion process in step (7) is become into 30min, 40min, 50min, 60min, 90min successively, its
His condition is same as Example 1.
After tested, it is 30min when the reaction time of corrosion process, it can be observed that complete flower-shaped ferrous acid can not be obtained
Bismuth, still can be observed the bismuth ferrite of a small amount of slab-like, but still be bismuth ferrite pure phase；It is 60min when the reaction time of corrosion process
During with 90min, complete flower-shaped bismuth ferrite can be obtained and nanometer sheet is thinner, but occur in that Bi25FeO40And Bi2O3Deng dephasign,
Therefore it is undesirable.And when the reaction time of corrosion process being 40min and 50min, XRD and SEM results are conformed to
Ask；When the reaction time of corrosion process being 40min, thing is still mutually bismuth ferrite, and slab-like bismuth ferrite is wholly absent, tentatively can be with
It is the regular of 45min to obtain flower-like structure but no reaction time；When the reaction time of corrosion process is 50min, the iron for obtaining
Sour bismuth flower-like structure is complete, regular and is evenly distributed, and XRD results are shown as bismuth ferrite pure phase but the crystallinity relative response time is
45min's is slightly poor.
Embodiment 3
N in step (7), N-dimethylformamide are become 60 successively with the volume ratio of hydrazine hydrate:4,80:4,100:4,
120:4, other conditions are same as Example 1.
After tested, when the volume ratio of DMF and hydrazine hydrate is 120:When 4, observed from SEM, not
Complete flower-shaped bismuth ferrite can be obtained, the bismuth ferrite of a small amount of slab-like still can be observed, XRD results show to be still pure bismuth ferrite
Phase；Work as N, N-dimethylformamide is 60 with the volume ratio of hydrazine hydrate:When 4, complete flower-shaped bismuth ferrite and nanometer sheet can be obtained
It is thinner, and occur in that Bi in XRD results25FeO40, Bi2O3And Bi2S3It is Deng dephasign therefore undesirable.And work as N, N dimethyl
Formamide is 80 with the volume ratio of hydrazine hydrate:4 and 100:When 4, XRD and SEM results meet the requirements；Work as N, N dimethyl formyl
Amine is 80 with the volume ratio of hydrazine hydrate:When 4, thing is still mutually bismuth ferrite, and slab-like bismuth ferrite is wholly absent, can tentatively be spent
Shape structure but not volume ratio are 90:4 it is regular；N, N-dimethylformamide is 100 with the volume ratio of hydrazine hydrate:When 4, obtain
Bismuth ferrite flower-like structure it is complete, regular and be evenly distributed, XRD results are shown as bismuth ferrite pure phase but crystallinity relative volume ratio
It is 90:4 it is poor.
From above test result and embodiment 2, the reaction time is short or ratio of DMF and hydrazine hydrate
When less, cause reaction not exclusively and complete flower-shaped spheroid can not be obtained, on the contrary condition can cause thing mutually to change again
Change then generates other bismuth ferriferous oxides.Therefore, DMF and the volume ratio of hydrazine hydrate are 90 in the present invention:4:
1, the reaction time is 45min, is optimum condition.
Embodiment 4
A kind of three-dimensional flower-shaped Bi2Fe4O9And preparation method thereof, comprise the following steps：
(1) according to Bi2Fe4O9In mol ratio weigh respectively mole be 1mmol Bi (NO3)3·5H2O, 2mmol
Fe (NO3)3·9H2O, 15mL water and 1mL concentrated nitric acids (65wt.%), magnetic agitation after mixing, make it fully dissolve and are mixed
Close liquid A；
(2) to being slowly added dropwise 45mL 10mol/L NaOH solutions in mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B is poured into ptfe autoclave, carries out homogeneous hydro-thermal reaction, reaction temperature is 180 DEG C,
Time is 12h；
(4) after question response kettle is cooled to room temperature, the precipitation that will be obtained after reaction passes through deionized water and absolute ethanol washing
Afterwards, it is put into 60 DEG C of baking oven and dries 12h, obtains bismuth ferrite powder；
(5) DMF of bismuth ferrite powder 3mg and 1mL is mixed in silk mouthful bottle, ultrasonic disperse 20min；
(6) heating water bath at silk mouthful bottle being placed in into 80 DEG C, and start stirring, it is passed through nitrogen；
(7) it is 4 to ratio is added dropwise in mixed liquor:1 hydrazine hydrate and methyl thioglycolate, nitrogen sustainable protection, instead
After 45min should being carried out, 0 DEG C of the rapid terminating reaction of cold ethanol is added；N in corrosion process, N-dimethylformamide：Hydrazine hydrate
Volume ratio is 90:4.
(8) sediment that will be obtained after reaction is put into 60 DEG C of dryings of baking oven after absolute ethyl alcohol and deionized water are washed
6h, obtains the bismuth ferrite powder of loose structure.
Embodiment 5
A kind of three-dimensional flower-shaped Bi2Fe4O9And preparation method thereof, comprise the following steps：
(1) according to Bi2Fe4O9In mol ratio weigh respectively mole be 1mmol Bi (NO3)3·5H2O, 2mmol
Fe (NO3)3·9H2O, 10mL water and 2mL concentrated nitric acids (65wt.%), magnetic agitation after mixing, make it fully dissolve and are mixed
Close liquid A；
(2) to being slowly added dropwise 50mL 10mol/L NaOH solutions in mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B is poured into ptfe autoclave, carries out homogeneous hydro-thermal reaction, reaction temperature is 200 DEG C,
Time is 10h；
(4) after question response kettle is cooled to room temperature, the precipitation that will be obtained after reaction passes through deionized water and absolute ethanol washing
Afterwards, it is put into 70 DEG C of baking oven and dries 10h, obtains bismuth ferrite powder；
(5) DMF of bismuth ferrite powder 2.5mg and 1mL is mixed in silk mouthful bottle, ultrasonic disperse
25min；
(6) heating water bath at silk mouthful bottle being placed in into 75 DEG C, and start stirring, it is passed through nitrogen；
(7) it is 4 to ratio is added dropwise in mixed liquor:1 hydrazine hydrate and methyl thioglycolate, nitrogen sustainable protection, instead
After 45min should being carried out, 2 DEG C of the rapid terminating reaction of cold ethanol is added；N in corrosion process, N-dimethylformamide：Hydrazine hydrate
Volume ratio is 90:4.
(8) sediment that will be obtained after reaction is put into 70 DEG C of dryings of baking oven after absolute ethyl alcohol and deionized water are washed
12h, obtains the bismuth ferrite powder of loose structure.
Embodiment 6
A kind of three-dimensional flower-shaped Bi2Fe4O9And preparation method thereof, comprise the following steps：
(1) according to Bi2Fe4O9In mol ratio weigh respectively mole be 1mmol Bi (NO3)3·5H2O, 2mmol
Fe (NO3)3·9H2O, 12mL water and 1.5mL concentrated nitric acids (65wt.%), magnetic agitation after mixing, make it fully dissolve and obtain
Mixed liquor A；
(2) to being slowly added dropwise 48mL 11mol/L NaOH solutions in mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B is poured into ptfe autoclave, carries out homogeneous hydro-thermal reaction, reaction temperature is 190 DEG C,
Time is 8h；
(4) after question response kettle is cooled to room temperature, the precipitation that will be obtained after reaction passes through deionized water and absolute ethanol washing
Afterwards, it is put into 80 DEG C of baking oven and dries 8h, obtains bismuth ferrite powder；
(5) DMF of bismuth ferrite powder 2.8mg and 1mL is mixed in silk mouthful bottle, ultrasonic disperse
30min；
(6) heating water bath at silk mouthful bottle being placed in into 70 DEG C, and start stirring, it is passed through nitrogen；
(7) it is 2 to ratio is added dropwise in mixed liquor:1 hydrazine hydrate and methyl thioglycolate, nitrogen sustainable protection, instead
After 45min should being carried out, the rapid terminating reaction of cold ethanol of 2 DEG C of ﹣ is added；N in corrosion process, N-dimethylformamide：Hydrazine hydrate
Volume ratio is 90:4.
(8) sediment that will be obtained after reaction is put into 80 DEG C of dryings of baking oven after absolute ethyl alcohol and deionized water are washed
8h, obtains the bismuth ferrite powder of loose structure.
By the exploration to photocatalysis performance, it can be found that adding the methyl orange sample of flower-shaped bismuth ferrite of the invention ultraviolet
Under light, can be degradable in 3 hours, and add the sample of bismuth ferrite before corrosion to be only degraded 20%.This can be construed to corrosion
The flower-like structure for obtaining afterwards contributes to the defect that the absorption of light and corrosion process are produced that some middle valence states occur, it helps
Electron transition is so as to improve the disposal efficiency.
Claims (10)
1. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder, it is characterised in that comprise the following steps：
Step 1：The bismuth ferrite powder of slab-like and corrosion solvent are pressed into (2.5~3) mg：1mL mixes, and carries out ultrasonic disperse, obtains
To mixed liquor A；
Step 2：Under protective atmosphere, mixed liquor A is carried out into heating water bath and is stirred, while to volume ratio is added dropwise in mixed liquor A
It is (2~4)：1 reducing agent and complexing agent, carry out corrosion reaction, wherein, corrosion solvent and reducing agent volume ratio for (80~
100)：4；Cooled down rapidly after 40~50min of reaction, terminating reaction；
Step 3：The sediment obtained after step 2 is reacted is washed and dried, and obtains three-dimensional flower-shaped bismuth ferrite powder.
2. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 1, it is characterised in that step 1
The preparation process of the bismuth ferrite powder of middle slab-like includes：
A () takes Bi (NO respectively3)3·5H2O、Fe(NO3)3·9H2O, water and nitric acid, magnetic agitation after mixing make it fully dissolve
Obtain mixed liquid B；Wherein, Bi (NO3)3·5H2O、Fe(NO3)3·9H2The ratio of O, water and nitric acid is 1mmol：2mmol：(10~
15)mL：(1~2) mL；
B () after obtaining suspension C russet, continues to stir to NaOH solution is slowly added dropwise in mixed liquid B；
C suspension C is poured into reactor and sealed by (), carry out homogeneous hydro-thermal reaction, generates sediment；
D () question response kettle is cooled to room temperature after, the sediment washing that homogeneous hydro-thermal reaction is obtained obtains slab-like after drying
Bismuth ferrite powder.
3. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
A the mass fraction of nitric acid is 65% in ()；The concentration of NaOH solution is 10~12mol/L in step (b), and drop rate is per second
Two drops.
4. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
C the condition of homogeneous hydro-thermal reaction is in ()：, at 180~200 DEG C, the reaction time is in 6~12h for reaction temperature.
5. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
D in (), then the sediment that homogeneous hydro-thermal reaction is obtained is dried by deionized water and absolute ethanol washing at 60~80 DEG C
8~12h.
6. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 1, it is characterised in that step 1
In, corrosion solvent is DMF；Reducing agent is hydrazine hydrate in step 2, and complexing agent is methyl thioglycolate.
7. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 1, it is characterised in that step 1
In, 20~30min of ultrasonic disperse.
8. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 1, it is characterised in that step 2
In, protective atmosphere is nitrogen or inert gas；Water bath heating temperature is 70~80 DEG C.
9. a kind of preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 1, it is characterised in that step 2
The supercooling absolute ethyl alcohol of middle use -2~2 DEG C carries out rapid cooling and terminates；Sediment absolute ethyl alcohol that corrosion reaction is obtained and
Deionized water is washed respectively until then pH dries 6~12h in neutrality at 60~80 DEG C.
10. a kind of three-dimensional flower-shaped bismuth ferrite powder, it is characterised in that the bismuth ferrite powder be nanometer sheet be self-assembly of it is straight
Three-dimensional flower-shaped sphere structure of the footpath at 1~2 μm.
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