CN106698521B - A kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof - Google Patents
A kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof, including：With Bi (NO3)3·5H2O and Fe (NO3)3·9H2O is initiation material, and block bismuth ferrite powder is prepared with hydro-thermal method, then under protective atmosphere, bismuth ferrite powder and corrosion solvent, reducing agent and complexing agent is mixed, the bismuth ferrite bouquet of three-dimensional porous structure is obtained through a step etch.The present invention prepares out raw material slab-like Bi using hydro-thermal method is gone out2Fe4O9Powder, grain size shape is uniformly and dispersiveness is preferable, then using etching process, preparation technology is simple to operate, and the cycle is short；The flower-shaped bismuth ferrite diameter prepared is about 1~2 μm, uniform in size, and because specific surface area is larger, the performance of each side is improved its loose structure.
Description
【Technical field】
The invention belongs to materials science field, 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, more 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 advantageous to reclaim with weak ferromagnetism.It effectively can be carried out using visible ray
Light-catalysed generation catalyst, there is application prospect in using energy source, wastewater treatment, purification of air etc..In addition, porous material
Application and conduct optics and nano-reactor in catalysis and separation also obtain people and more and more paid 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 obtain the crystal of the submicron-scale of favorable dispersibility.By adjusting mineralising agent concentration, can obtain
Obtain laminar, tabular and cube block crystal；Under the conditions of high KOH concentration (12M), 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, is corroded by a step
Method, prepare the three-dimensional flower-shaped bismuth ferrite powder with high specific surface area.
For achieving the above object, the present invention adopts 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 is mixed, and carries out ultrasound point
Dissipate, obtain mixed liquor A；
Step 2：Under protective atmosphere, mixed liquor A is subjected to heating water bath and stirred, while body is added dropwise into mixed liquor A
Product ratio is (2~4)：1 reducing agent and complexing agent, corrosion reaction is carried out, wherein, the volume ratio for corroding 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) Bi (NO are taken 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)3·9H2O, the ratio of water and nitric acid is 1mmol：2mmol：
(10~15) mL：(1~2) mL；
(b) NaOH solution is slowly added dropwise into mixed liquid B, after obtaining suspension C russet, continues to stir；
(c) suspension C is poured into reactor and sealed, carry out homogeneous hydro-thermal reaction, generate sediment；
(d) after question response kettle is cooled to room temperature, sheet is obtained after the sediment washing that homogeneous hydro-thermal reaction obtains is dried
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 are per second two drops.
Further, the condition of homogeneous hydro-thermal reaction is in step (c)：Reaction temperature is at 180~200 DEG C, the reaction time
In 6~12h.
Further, in step (d), the sediment that homogeneous hydro-thermal reaction obtains 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 in step 2, complexing
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 obtains
To sediment with 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 the three-dimensional flower-shaped sphere structure of diameter that nanometer sheet is self-assembly of 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, corrosion process is then carried out by a step etch, three-dimensional flower-shaped Bi is made2Fe4O9Powder, increase
Big Bi2Fe4O9Specific surface area, Bi before and after corrosion2Fe4O9Specific 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, be advantageous to Bi2Fe4O9Crystal grain is big
Small shape is uniformly and dispersiveness is preferable.The present invention uses etching process, and the grain dispersion after corrosion is uniform, and used in preparation
Condition can be controlled preferably.The present invention obtains three-dimensional flower ball-shaped Bi2Fe4O9Method it is novel, particle is uniformly and equipment is grasped
It is required that low, technique is simple, energy consumption is low, can operate continuously and process condition is easily controlled.
Three-dimensional flower-shaped Bi produced by the present invention2Fe4O9Powder purity is high, crystallinity is good, pattern is uniform, and what is obtained is
The flower-like structure that a kind of nanometer sheet is self-assembly of, diameter are 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.
【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 to weigh mol ratio respectively be 1mmol：2mmol Bi (NO3)3·5H2O,
Fe(NO3)3·9H2O, 10~15mL water and 1~2mL concentrated nitric acids (65wt.%) are measured, magnetic agitation after mixing, makes it fully molten
Solution obtains mixed liquor A；Add concentrated nitric acid purpose can be completely dissolved in the nitrate in bismuth and iron 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) 45~50mL, 10~12mol/L NaOH solution is added dropwise with the speed of per second two drops into mixed liquor A,
With precipitate B i3+And Fe3+, after obtaining suspension B russet, continue to stir；NaOH concentration in 10~12mol/L scope,
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, it is anti-to carry out homogeneous hydro-thermal
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 obtained after reaction is washed by deionized water and absolute ethyl alcohol
Afterwards, 8~12h is dried at 60~80 DEG C in vacuum drying chamber, obtains bismuth ferrite powder.
5) bismuth ferrite powder obtained in step 4) and DMF are mixed in silk mouth bottle, ultrasonic disperse
20~30min；Bismuth ferrite powder and N, the mass volume ratio of N-dimethylformamide is 2.5~3mg：1mL.
6) silk mouth bottle is subjected to heating water bath and stirred, water bath heating temperature is 70~80 DEG C, while is passed through nitrogen and continues
Protection；
7) volume ratio is added dropwise into mixed liquor as 2~4:1 hydrazine hydrate and methyl thioglycolate, nitrogen are persistently protected
Shield, after reaction carries out 40~50min, add -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) after the sediment obtained after reaction is washed by absolute ethyl alcohol and deionized water, 6 are dried at 60~80 DEG C
~12h, obtain 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, methyl thioglycolate oxidation deactivation is avoided, wherein nitrogen cost is low, and liquid nitrogen storage gets up and more pacified
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 using 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, the bismuth ferrite of slab-like is peeled off into nanometer sheet, these final nanometer sheets pass through 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, uniform in size, compared to its ratio of the slab-like bismuth ferrite before corrosion
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) 45mL 10mol/L NaOH solutions are slowly added dropwise into mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B to be 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 obtained after reaction is washed by deionized water and absolute ethyl alcohol
Afterwards, the dry 12h of 60 DEG C of baking oven is put into, obtains bismuth ferrite powder；
(5) bismuth ferrite powder 3mg and 1mL DMF are mixed in silk mouth bottle, ultrasonic disperse 20min；
(6) silk mouth bottle is placed in heating water bath at 80 DEG C, and starts to stir, be passed through nitrogen；
(7) ratio is added dropwise into mixed liquor as 4:1 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) after the sediment obtained after reaction is washed by absolute ethyl alcohol and deionized water, 60 DEG C of dryings of baking oven are put into
6h, obtain the bismuth ferrite powder of loose structure.
Fig. 1 and Fig. 2 is respectively the XRD of bismuth ferrite before and after corroding under the reaction condition, it can be seen that prepared by hydro-thermal method
Bi2Fe4O9Generated without dephasign, crystallinity is preferable, the Bi after being handled by a step corrosion process2Fe4O9Still generated without dephasign.It is and rotten
Bi after erosion2Fe4O9It is obvious before diffraction peak intensity is relatively corrosive to reduce.Fig. 3 and Fig. 4 is respectively before and after corroding under 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
200nm or so slab-like is spent, surface is smooth and smooth, and shape is uniform, favorable dispersibility；After being handled by a step corrosion process
Obtained Bi2Fe4O9It 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 is 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 Bi occur25FeO40And Bi2O3Deng dephasign,
Therefore it is undesirable.And when the reaction time of corrosion process is 40min and 50min, XRD and SEM results conform to
Ask；When the reaction time of corrosion process is 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 do not have the reaction time；When the reaction time of corrosion process is 50min, obtained iron
Sour bismuth flower-like structure is complete, regular and be 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
By N in step (7), the volume ratio of N-dimethylformamide and hydrazine hydrate becomes 60 successively: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 that bismuth ferrite is pure
Phase；Work as N, the volume ratio of N-dimethylformamide and hydrazine hydrate is 60:When 4, complete flower-shaped bismuth ferrite and nanometer sheet can be obtained
It is thinner, and there is Bi in XRD results25FeO40, Bi2O3And Bi2S3Deng dephasign, thus it is undesirable.And work as N, N dimethyl
The volume ratio of formamide and hydrazine hydrate is 80:4 and 100:When 4, XRD and SEM results meet the requirements；Work as N, N dimethyl formyl
The volume ratio of amine and hydrazine hydrate is 80:When 4, thing is still mutually bismuth ferrite, and slab-like bismuth ferrite is wholly absent, can tentatively spent
Shape structure but without volume ratio be 90:4 it is regular；The volume ratio of N, N-dimethylformamide and hydrazine hydrate is 100: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
For 90:4 it is poor.
From above test result and embodiment 2, the reaction time is short or the ratio of DMF and hydrazine hydrate
When less, cause reaction not exclusively and complete flower-shaped spheroid can not be obtained, condition is on the contrary to cause thing mutually to change again
Change then generates other bismuth ferriferous oxides.Therefore, the volume ratio of DMF and hydrazine hydrate is 90 in the present invention:4:
1, reaction time 45min, it 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) 45mL 10mol/L NaOH solutions are slowly added dropwise into mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B to be 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 obtained after reaction is washed by deionized water and absolute ethyl alcohol
Afterwards, the dry 12h of 60 DEG C of baking oven is put into, obtains bismuth ferrite powder；
(5) bismuth ferrite powder 3mg and 1mL DMF are mixed in silk mouth bottle, ultrasonic disperse 20min；
(6) silk mouth bottle is placed in heating water bath at 80 DEG C, and starts to stir, be passed through nitrogen；
(7) ratio is added dropwise into mixed liquor as 4:1 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) after the sediment obtained after reaction is washed by absolute ethyl alcohol and deionized water, 60 DEG C of dryings of baking oven are put into
6h, obtain 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) 50mL 10mol/L NaOH solutions are slowly added dropwise into mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B to be 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 obtained after reaction is washed by deionized water and absolute ethyl alcohol
Afterwards, the dry 10h of 70 DEG C of baking oven is put into, obtains bismuth ferrite powder；
(5) bismuth ferrite powder 2.5mg and 1mL DMF are mixed in silk mouth bottle, ultrasonic disperse
25min；
(6) silk mouth bottle is placed in heating water bath at 75 DEG C, and starts to stir, be passed through nitrogen；
(7) ratio is added dropwise into mixed liquor as 4:1 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) after the sediment obtained after reaction is washed by absolute ethyl alcohol and deionized water, 70 DEG C of dryings of baking oven are put into
12h, obtain 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 to obtain
Mixed liquor A；
(2) 48mL 11mol/L NaOH solutions are slowly added dropwise into mixed liquor A, after obtaining suspension B russet, after
Continuous stirring；
(3) suspension B to be 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 obtained after reaction is washed by deionized water and absolute ethyl alcohol
Afterwards, the dry 8h of 80 DEG C of baking oven is put into, obtains bismuth ferrite powder；
(5) bismuth ferrite powder 2.8mg and 1mL DMF are mixed in silk mouth bottle, ultrasonic disperse
30min；
(6) silk mouth bottle is placed in heating water bath at 70 DEG C, and starts to stir, be passed through nitrogen；
(7) ratio is added dropwise into mixed liquor as 2:1 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) after the sediment obtained after reaction is washed by absolute ethyl alcohol and deionized water, 80 DEG C of dryings of baking oven are put into
8h, obtain the bismuth ferrite powder of loose structure.
By the exploration to photocatalysis performance, it can be found that adding the methyl orange sample of the flower-shaped bismuth ferrite of the present invention ultraviolet
, can be degradable in 3 hours under light, and the sample for adding bismuth ferrite before corrosion is only degraded 20%.This can be construed to corrode
The flower-like structure obtained afterwards contributes to the defects of absorption of light and corrosion process generation that some middle valence states occur, it helps
Electron transition is so as to improving 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 is mixed, and is carried out ultrasonic disperse, is obtained
To mixed liquor A；
Step 2：Under protective atmosphere, mixed liquor A is subjected to heating water bath and stirred, while volume ratio is added dropwise into mixed liquor A
For (2~4)：1 reducing agent and complexing agent, carry out corrosion reaction, wherein, corrode the volume ratio of solvent and reducing agent 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.
A kind of 2. 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) Bi (NO are taken 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)3·9H2O, the ratio of water and nitric acid is 1mmol：2mmol：(10~
15)mL：(1~2) mL；
(b) NaOH solution is slowly added dropwise into mixed liquid B, after obtaining suspension C russet, continues to stir；
(c) suspension C is poured into reactor and sealed, carry out homogeneous hydro-thermal reaction, generate sediment；
(d) after question response kettle is cooled to room temperature, slab-like is obtained after the sediment washing that homogeneous hydro-thermal reaction obtains is dried
Bismuth ferrite powder.
A kind of 3. preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
(a) 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.
A kind of 4. preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
(c) condition of homogeneous hydro-thermal reaction is in：Reaction temperature is at 180~200 DEG C, and the reaction time is in 6~12h.
A kind of 5. preparation method of three-dimensional flower-shaped bismuth ferrite powder according to claim 2, it is characterised in that step
(d) in, the sediment that homogeneous hydro-thermal reaction obtains is washed by deionized water and absolute ethyl alcohol, is then dried at 60~80 DEG C
8~12h.
A kind of 6. 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.
A kind of 7. 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.
A kind of 8. 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.
A kind of 9. 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 terminated；Sediment absolute ethyl alcohol that corrosion reaction obtains and
Deionized water is washed respectively until then pH dries 6~12h in neutrality at 60~80 DEG C.
10. a kind of utilize bismuth ferrite powder three-dimensional flower-shaped made from preparation method described in claim 1, it is characterised in that should
Bismuth ferrite powder is the three-dimensional flower-shaped Bi of diameter that nanometer sheet is self-assembly of at 1~2 μm2Fe4O9Sphere structure.
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| CN107960050A (en) * | 2017-12-12 | 2018-04-24 | 陕西科技大学 | A kind of preparation method of graphene/three-dimensional flower-shaped bismuth ferrite composite wave-suction material |
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| 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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| CN114084911B (en) * | 2021-11-04 | 2023-12-22 | 江苏科技大学 | Bi (Bi) 2 Fe 4 O 9 Preparation method and application of material |
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