CN109437317A - A kind of flower-shaped BiFeO of hydro-thermal method preparation3Powder and preparation method thereof - Google Patents
A kind of flower-shaped BiFeO of hydro-thermal method preparation3Powder and preparation method thereof Download PDFInfo
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Abstract
A kind of flower-shaped BiFeO of hydro-thermal method preparation of the present invention3Powder and preparation method thereof, the method includes, steps 1 to press 1:(1~1.1) molar ratio is by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in nitric acid, obtains Fe3+Concentration is female salting liquid of 0.13~0.17mol/L；Step 2, it is 11~13 with the pH that NaOH solution adjusts female salting liquid, obtains the mixed system A containing reddish brown precipitation；Step 3, the reddish brown precipitation in mixed system A is washed after cleaning solution is in neutrality, and the presoma powder of hydro-thermal is obtained by filtration；Step 4, it is 12~13 with the pH that NaOH solution adjusts hydro-thermal presoma powder, obtains mixed system B, mixed system B carries out washed product after 8~16h of hydro-thermal reaction at 180~200 DEG C, cleaning solution after to washing is in neutrality, and obtains flower-shaped BiFeO after resulting product drying3Powder.
Description
Technical field
The present invention relates to hydro-thermal methods to prepare powder technology field, specially a kind of flower-shaped BiFeO of hydro-thermal method preparation3Powder
And preparation method thereof.
Background technique
With the continuous development of information technology, the miniaturization of device and multifunction make people show characteristic to a variety of objects are collected
The interest of multifunctional material research is constantly surging, and multi-ferroic material be exactly in a kind of material simultaneously there are two types of tools or
The functional material of two or more primary ferroics, wherein the primary ferroic includes ferromagnetic, ferroelectricity, iron rotation and ferroelasticity
Deng.Recent years, in multi-iron material Subcommittee-to studies carefully, people largely focus on containing two kinds of primary iron of ferromagnetism and ferroelectricity
Material, this material and it is magnetic orderly and ferroelectric order, wherein it is magnetic orderly include ferromagnetism, ferrimagnetism, anti-ferromagnetism with
And weak ferromagnetism caused by being tilted by antiferromagnetic rotation, then, under the action of external electric field or external magnetic field, polarization and magnetized direction
It can invert, while the existing effect of intercoupling between magnetization vector and polarization vector, so that external electric field can be with
Change the magnetized state of material, same external magnetic field also can change its polarized state, this is just the novel design for being threaded onto and learning device
Provide a new freedom degree.
BiFeO3It is few in number can have ferroelectricity/anti-ferromagnetic single-phase iron electromagnet material, ferroelectricity at room temperature
The Curie temperature of phase transformation is 1103K, and the Neel temperature of antiferromagnetic phase transformation is 643K.Currently, preparation BiFeO3The method of powder exists
It is reported in the literature very much, such as high temperature solid-state method, sol-gel method and chemical coprecipitation.The above method is often difficult
To the BiFeO of pure phase3, especially high temperature solid-state method not only needs to remove Bi by nitric acid after the sintering2Fe4O9With
Bi25FeO40Etc. impurity phases, keep powder surface coarse, the repeatability of experiment is also bad, and synthesis temperature is higher, often connects
Closely it is even higher than Curie temperature and Neel temperature, the final ferroelectric properties and ferromagnetic property for influencing material.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of flower-shaped BiFeO of hydro-thermal method preparation3Powder and its
Preparation method, simple process, low in cost, reaction time is short, reproducible, the BiFeO prepared3Powder not only partial size it is small and
And narrow distribution range.
The present invention is to be achieved through the following technical solutions:
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps:
Step 1, solution is configured, by 1:(1~1.1) molar ratio by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in
In nitric acid, Fe is obtained3+Concentration is female salting liquid of 0.13~0.17mol/L；
Step 2, it is 11~13 with the pH that NaOH solution adjusts female salting liquid, obtains the mixed system containing reddish brown precipitation
A；
Step 3, the reddish brown precipitation in mixed system A is washed after cleaning solution is in neutrality, before hydro-thermal is obtained by filtration
Drive body powder；
Step 4, it is 12~13 with the pH that NaOH solution adjusts hydro-thermal presoma powder, mixed system B is obtained, by mixture
It is that B carries out washed product after 8~16h of hydro-thermal reaction at 180~200 DEG C, until the cleaning solution after washing is in neutrality, resulting production
Flower-shaped BiFeO is obtained after object drying3Powder.
Preferably, nitric acid described in step 1 is concentrated nitric acid, and the volume of concentrated nitric acid is 4~30mL.
Preferably, the pH of female salting liquid is adjusted in the step 2 using the method stirred when NaOH solution is added dropwise,
The titration speed of NaOH solution is 1~2mL/min.
Preferably, the step 2 first stirs 30~60min after obtaining reddish brown precipitation, then stands 1~2h and obtain
Mixed system A containing reddish brown precipitation.
Preferably, mixed system B is transferred in reaction kettle by the step 4 carries out hydro-thermal reaction, the filling rate of reaction kettle
It is 75~85%.
Preferably, the heating rate that mixed system B reaches reaction temperature in the step 4 is 1~2 DEG C/min.
Preferably, mixed system B after the reaction, is washed with deionized product 4~5 times in the step 4, until after washing
Cleaning solution be in neutrality, then obtain product after washing 2~3 2~4h of standing with dehydrated alcohol.
Preferably, the resulting product of the step 4 obtains flower-shaped BiFeO after 50~80 DEG C of 12~15h of drying3Powder.
Preferably, Fe (NO in the step 13)3·9H2O and Bi (NO3)3·5H2The molar ratio of O be 1:(1.02~
1.07) Fe, is obtained3+Concentration is female salting liquid of 0.14~0.16mol/L.
A kind of flower-shaped BiFeO that the method as described in above-mentioned any one is prepared3Powder.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention prepares flower-shaped BiFeO3The method of powder, Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in HNO3It can
To avoid introducing foreign ion；The pH that NaOH solution adjusts female salting liquid is 11~13 available Fe (OH)3With Bi (OH)3It is mixed
The reddish brown precipitation of conjunction, the solution in mixed system A, which is in neutrality, can guarantee to obtain pure Fe (OH)3With Bi (OH)3Precipitating, does not have
There is NO3 —Be mixed into, BiFeO can have been arrived after hydro-thermal reaction3, NaOH and H2The mixed liquor of O, washing to the cleaning solution after washing are in
Property simultaneously dries BiFeO3Obtain the flower-shaped BiFeO that partial size is 1 μm or so3Powder.The present invention successfully prepares a kind of with flower-like structure
BiFeO3Powder, powder are to be piled into flower by piece.
Further, reaction process can be made by extraneous shadow using the compactedness and heating rate of precursor liquid in control reaction kettle
It rings and reduces, make preparation process that there is repeatability well.
Detailed description of the invention
Fig. 1 is flower-shaped BiFeO prepared by the embodiment of the present invention 13The XRD diagram of powder.
Fig. 2 is flower-shaped BiFeO prepared by the embodiment of the present invention 13The SEM of powder schemes.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Hydrothermal synthesis method of the present invention, can compared with high temperature solid-state method, sol-gel method, chemical coprecipitation
To carry out at a lower temperature, resulting BiFeO3Powder has good crystallization, dispersing characteristic, has big specific surface area
And surface-active, obtain the BiFeO of pure phase3Powder.
Embodiment 1
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps,
Step 1, solution is configured:
Fe (NO is weighed by the molar ratio of 1:1.053)3·9H2O and Bi (NO3)3·5H2O is dissolved in the dense HNO of 5mL3In
Obtain Fe3+Concentration is female salting liquid of 0.15mol/L, wherein female salting liquid is referred to comprising Fe (NO3)3·9H2O、Bi
(NO3)3·5H2O and dense HNO3Mixed solution；
Step 2, NaOH solution is added dropwise while stirring into female salting liquid, rate of titration 1mL/min is added dropwise to pH=
12, reddish brown precipitation is obtained, is continued after stirring 30min, 2h is stood and obtains the mixed system A containing reddish brown precipitation；
Step 3, with the reddish brown precipitation in the deionized water mixed system A that washing step 2 obtains repeatedly, make mixed system
Cleaning solution in A is in neutrality, and supernatant is removed by the way of filtering, obtains hydro-thermal method preparation BiFeO3Required precursor
Body；
Step 4, the pH that NaOH solution to solution as mineralizer is added dropwise while stirring into presoma powder is 12, will
Solution is transferred in reaction kettle, filling rate 80%, and heating rate is 1 DEG C/min, and reaction temperature is 200 DEG C, and the reaction time is
12h；
Step 5, it takes out and is washed with deionized after solution after reaction during the product 4 times cleaning solutions to after washing are in
Property after stand 2h, then after washing 2 times with dehydrated alcohol, product is dried to the BiFeO that rhombohedral system is obtained after 15h at 50 DEG C3
Powder, crystalline structure R3C.BiFeO obtained by the present embodiment3Powder average particle diameter size is 1~1.5 μm.Its XRD diagram
As shown in Figure 1, it can be seen from the figure that prepared BiFeO3Powder is pure rhombohedral system, without the generation of other miscellaneous phases.
SEM figure is as shown in Fig. 2, it can be seen from the figure that the BiFeO of preparation3The pattern of powder be it is flower-shaped, average particle diameter size be 1~
1.5μm。
Embodiment 2
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps,
Step 1, solution is configured；
Fe (NO is weighed by the molar ratio of 1:1.023)3·9H2O and Bi (NO3)3·5H2O is dissolved in the dense HNO of 24mL3In
Obtain Fe3+Concentration is female salting liquid of 0.13mol/L；
Step 2, NaOH solution is added dropwise while stirring into female salting liquid, rate of titration 1.7mL/min is added dropwise to pH=
12, reddish brown precipitation is obtained, is continued after stirring 30min, 2h is stood and obtains the mixed system A containing reddish brown precipitation；
Step 3, with the reddish brown precipitation in the deionized water mixed system A that washing step 2 obtains repeatedly, make mixed system
Cleaning solution in A is in neutrality, and supernatant is removed by the way of filtering, obtains hydro-thermal method preparation BiFeO3Required precursor
Body；
Step 4, being added dropwise while stirring into presoma powder as NaOH solution to the pH value of solution of mineralizer is 12, will be molten
Liquid is transferred in reaction kettle, filling rate 80%, and heating rate is 1 DEG C/min, and reaction temperature is 180 DEG C, reaction time 8h；
Step 5, it takes out and is washed with deionized after solution after reaction during the product 4 times cleaning solutions to after washing are in
2h is stood after property, then after washing 2 times with dehydrated alcohol, obtains BiFeO after product is dried 15h at 60 DEG C3Powder, it is obtained
BiFeO3Powder average particle diameter size is 1.5~2 μm.
Embodiment 3
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps,
Step 1, solution is configured；
Fe (NO is weighed by the molar ratio of 1:13)3·9H2O and Bi (NO3)3·5H2O is dissolved in the dense HNO of 18mL3In
To Fe3+Concentration is female salting liquid of 0.14mol/L；
Step 2, NaOH solution is added dropwise while stirring into female salting liquid, rate of titration 1.2mL/min is added dropwise to pH=
11, reddish brown precipitation is obtained, is continued after stirring 40min, 1h is stood and obtains the mixed system A containing reddish brown precipitation；
Step 3, with the reddish brown precipitation in the deionized water mixed system A that washing step 2 obtains repeatedly, make mixed system
Cleaning solution in A is in neutrality, and supernatant is removed by the way of filtering, obtains hydro-thermal method preparation BiFeO3Required precursor
Body；
Step 4, being added dropwise while stirring into presoma powder as NaOH solution to the pH value of solution of mineralizer is 12.5, will
Solution is transferred in reaction kettle, filling rate 75%, and heating rate is 1.5 DEG C/min, and reaction temperature is 185 DEG C, the reaction time
For 10h；
Step 5, it takes out and is washed with deionized after solution after reaction during the product 5 times cleaning solutions to after washing are in
3h is stood after property, then after washing 2 times with dehydrated alcohol, obtains BiFeO after product is dried 14h at 70 DEG C3Powder.It is obtained
BiFeO3Powder average particle diameter size is at 2 μm or so.
Embodiment 4
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps,
Step 1, solution is configured；
Fe (NO is weighed by the molar ratio of 1:1.073)3·9H2O and Bi (NO3)3·5H2O is dissolved in the dense HNO of 10mL3In
Obtain Fe3+Concentration is female salting liquid of 0.16mol/L；
Step 2, NaOH solution is added dropwise while stirring into female salting liquid, rate of titration 1.5mL/min is added dropwise to pH=
11, reddish brown precipitation is obtained, is continued after stirring 50min, 1h is stood and obtains the mixed system A containing reddish brown precipitation；
Step 3, with the reddish brown precipitation in the deionized water mixed system A that washing step 2 obtains repeatedly, make mixed system
Cleaning solution in A is in neutrality, and supernatant is removed by the way of filtering, obtains hydro-thermal method preparation BiFeO3Required precursor
Body；
Step 4, being added dropwise while stirring into presoma powder as NaOH solution to the pH value of solution of mineralizer is 13, will be molten
Liquid is transferred in reaction kettle, filling rate 85%, and heating rate is 1.5 DEG C/min, and reaction temperature is 190 DEG C, and the reaction time is
14h；
Step 5, it takes out and is washed with deionized after solution after reaction during the product 5 times cleaning solutions to after washing are in
3h is stood after property, then after washing 3 times with dehydrated alcohol, obtains BiFeO after product is dried 12h at 80 DEG C3Powder.It is obtained
BiFeO3Powder average particle diameter size is at 2.5 μm or so.
Embodiment 5
A kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, includes the following steps,
Step 1, solution is configured；
Fe (NO is weighed by the molar ratio of 1:1.13)3·9H2O and Bi (NO3)3·5H2O is dissolved in the dense HNO of 30mL3In
Obtain Fe3+Concentration is female salting liquid of 0.17mol/L；
Step 2, NaOH solution is added dropwise while stirring into female salting liquid, rate of titration 2mL/min is added dropwise to pH=
13, reddish brown precipitation is obtained, is continued after stirring 60min, 1h is stood and obtains the mixed system A containing reddish brown precipitation；
Step 3, with the reddish brown precipitation in the deionized water mixed system A that washing step 2 obtains repeatedly, make mixed system
Cleaning solution in A is in neutrality, and supernatant is removed by the way of filtering, obtains hydro-thermal method preparation BiFeO3Required precursor
Body；
Step 4, the pH that NaOH solution to solution as mineralizer is added dropwise while stirring into presoma powder is 13, will
Solution is transferred in reaction kettle, filling rate 85%, and heating rate is 2 DEG C/min, and reaction temperature is 195 DEG C, and the reaction time is
16h；
Step 5, it takes out and is washed with deionized after solution after reaction during the product 5 times cleaning solutions to after washing are in
4h is stood after property, then after washing 3 times with dehydrated alcohol, obtains BiFeO after product is dried 13h at 80 DEG C3Powder.It is obtained
BiFeO3Powder average particle diameter size is at 3 μm or so.
Claims (10)
1. a kind of hydro-thermal method prepares flower-shaped BiFeO3The method of powder, which comprises the steps of:
Step 1, solution is configured, by 1:(1~1.1) molar ratio by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in nitric acid
In, obtain Fe3+Concentration is female salting liquid of 0.13~0.17mol/L；
Step 2, it is 11~13 with the pH that NaOH solution adjusts female salting liquid, obtains the mixed system A containing reddish brown precipitation；
Step 3, the reddish brown precipitation in mixed system A is washed after cleaning solution is in neutrality, and the presoma of hydro-thermal is obtained by filtration
Powder；
Step 4, it is 12~13 with the pH that NaOH solution adjusts hydro-thermal presoma powder, mixed system B is obtained, by mixed system B
The washed product after progress 8~16h of hydro-thermal reaction at 180~200 DEG C, until the cleaning solution after washing is in neutrality, resulting product
Flower-shaped BiFeO is obtained after drying3Powder.
2. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that step 1
Described in nitric acid be concentrated nitric acid, the volume of concentrated nitric acid is 4~30mL.
3. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
Step 2 in the pH of mother's salting liquid is adjusted using the method that stir when NaOH solution is added dropwise, the titration speed of NaOH solution is 1
~2mL/min.
4. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
Step 2 after obtaining reddish brown precipitation, first stir 30~60min, then stand 1~2h and obtain the mixing containing reddish brown precipitation
System A.
5. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
Mixed system B is transferred in reaction kettle and carries out hydro-thermal reaction by step 4, and the filling rate of reaction kettle is 75~85%.
6. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
It is 1~2 DEG C/min that mixed system B, which reaches the heating rate of reaction temperature, in step 4.
7. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
Mixed system B after the reaction, is washed with deionized product 4~5 times in step 4, until the cleaning solution after washing is in neutrality, then uses
Dehydrated alcohol obtains product after washing 2~3 2~4h of standing.
8. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
The resulting product of step 4 obtains flower-shaped BiFeO after 50~80 DEG C of 12~15h of drying3Powder.
9. a kind of hydro-thermal method according to claim 1 prepares flower-shaped BiFeO3The method of powder, which is characterized in that described
Fe (NO in step 13)3·9H2O and Bi (NO3)3·5H2The molar ratio of O is 1:(1.02~1.07), obtain Fe3+Concentration is 0.14
Female salting liquid of~0.16mol/L.
10. a kind of flower-shaped BiFeO that the method as described in any one of claim 1~9 is prepared3Powder.
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| CN111410237A (en) * | 2020-05-09 | 2020-07-14 | 中南林业科技大学 | Resource utilization method for waste polluted biomass |
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