CN109437317B - Flower-shaped BiFeO prepared by hydrothermal method3Powder and preparation method thereof - Google Patents
Flower-shaped BiFeO prepared by hydrothermal method3Powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to flower-shaped BiFeO prepared by a hydrothermal method3The powder and the preparation method thereof comprise the step 1 of mixing Fe (NO) according to the molar ratio of 1 (1-1.1)3)3·9H2O and Bi (NO)3)3·5H2Dissolving O in nitric acid to obtain Fe3+Mother salt solution with the concentration of 0.13-0.17 mol/L; step 2, adjusting the pH value of the mother salt solution to 11-13 by using a NaOH solution to obtain a mixed system A containing a brownish red precipitate; step 3, washing the brownish red precipitate in the mixed system A until the washing liquid is neutral, and filtering to obtain hydrothermal precursor powder; step 4, regulating the pH value of the hydrothermal precursor powder to 12-13 by using a NaOH solution to obtain a mixed system B, carrying out hydrothermal reaction on the mixed system B at 180-200 ℃ for 8-16 h, washing the product until the washed washing liquid is neutral, and drying the obtained product to obtain flower-shaped BiFeO3And (3) powder.
Description
Technical Field
The invention relates to the technical field of powder preparation by a hydrothermal method, in particular to flower-shaped BiFeO prepared by the hydrothermal method3Powder and a preparation method thereof.
Background
With the continuous development of information technology, the miniaturization and multi-functionalization of devices make people have an increasing interest in the research of multifunctional materials that integrate a plurality of current characteristics, and a multiferroic material is a functional material that has two or more primary ferrosofcs simultaneously in one material, wherein the primary ferrosofcs include ferromagnetism, ferroelectrics, ferroelasticity, and the like. In recent years, in the study of multi-iron materials, much attention has been paid to a material containing two primary ferroelectrics, namely ferromagnetism and ferroelectrics, which have both magnetic ordering and ferroelectric ordering, wherein the magnetic ordering includes ferromagnetism, ferrimagnetism, antiferromagnetism and weak ferromagnetism caused by antiferromagnetic spin tilt, so that under the action of an external electric field or an external magnetic field, the directions of polarization and magnetization can be reversed, and meanwhile, due to the mutual coupling effect between a magnetization vector and a polarization vector, the external electric field can change the magnetization state of the material, and the external magnetic field can also change the polarization state of the material, thereby providing a new degree of freedom for the design of a novel rotation-oriented chemical device.
BiFeO3The material is a few single-phase ferroelectric materials which can have ferroelectric/antiferromagnetic property at room temperature, the Curie temperature of the ferroelectric phase transition is 1103K, and the Neille temperature of the antiferromagnetic phase transition is 643K. Currently, BiFeO is prepared3Methods for powders are reported in the literature, for example, high temperature solid phase methods, sol-gel methods, and chemical coprecipitation methods. The above method often makes it difficult to obtain pure phase BiFeO3In particular high-temperature solid-phase methods, require not only the removal of Bi by means of nitric acid after sintering2Fe4O9And Bi25FeO40The surface of the powder is rough due to the impurity phases, the experimental repeatability is not good, the synthesis temperature is high and is often close to or even higher than the Curie temperature and the Neille temperature, and the ferroelectric property and the ferromagnetic property of the material are finally influenced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides flower-shaped BiFeO prepared by a hydrothermal method3The powder and the preparation method thereof have the advantages of simple process, low cost, short reaction period and good repeatability, and the prepared BiFeO3The powder has small particle size and narrow distribution range.
The invention is realized by the following technical scheme:
method for preparing flower-shaped BiFeO by hydrothermal method3The powder preparation method comprises the following steps:
step 1, preparing a solution, and adding Fe (NO) according to a molar ratio of 1 (1-1.1)3)3·9H2O and Bi (NO)3)3·5H2Dissolving O in nitric acid to obtain Fe3+Mother salt solution with the concentration of 0.13-0.17 mol/L;
step 2, adjusting the pH value of the mother salt solution to 11-13 by using a NaOH solution to obtain a mixed system A containing a brownish red precipitate;
step 3, washing the brownish red precipitate in the mixed system A until the washing liquid is neutral, and filtering to obtain hydrothermal precursor powder;
step 4, regulating the pH value of the hydrothermal precursor powder to 12-13 by using a NaOH solution to obtain a mixed system B, carrying out hydrothermal reaction on the mixed system B at 180-200 ℃ for 8-16 h, washing the product until the washed washing liquid is neutral, and drying the obtained product to obtain flower-shaped BiFeO3And (3) powder.
Preferably, the nitric acid in the step 1 is concentrated nitric acid, and the volume of the concentrated nitric acid is 4-30 mL.
Preferably, in the step 2, the pH of the mother salt solution is adjusted by a method of dripping NaOH solution while stirring, and the titration rate of the NaOH solution is 1-2 mL/min.
Preferably, after the brownish red precipitate is obtained in the step 2, the mixture is stirred for 30-60 min and then kept stand for 1-2 h to obtain a mixed system A containing the brownish red precipitate.
Preferably, in the step 4, the mixed system B is transferred to a reaction kettle for hydrothermal reaction, and the filling rate of the reaction kettle is 75-85%.
Preferably, the heating rate of the mixed system B reaching the reaction temperature in the step 4 is 1-2 ℃/min.
Preferably, after the reaction of the mixed system B in the step 4, the product is washed by deionized water for 4-5 times until the washed washing liquid is neutral, and then washed by absolute ethyl alcohol for 2-3 times and kept stand for 2-4 hours to obtain the product.
Preferably, the product obtained in the step 4 is dried at 50-80 ℃ for 12-15 h to obtain flower-shaped BiFeO3And (3) powder.
Preferably, Fe (NO) in said step 13)3·9H2O and Bi (NO)3)3·5H2The molar ratio of O is 1 (1.02-1.07), and Fe is obtained3+The concentration is 0.14 ℃ -0.16mol/L mother salt solution.
Flower-shaped BiFeO prepared by any one of the methods3And (3) powder.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention prepares flower-shaped BiFeO3Method of powder, Fe (NO)3)3·9H2O and Bi (NO)3)3·5H2O dissolved in HNO3Impurity ions can be prevented from being introduced; adjusting the pH of the mother salt solution to 11-13 with NaOH solution to obtain Fe (OH)3And Bi (OH)3Mixed brownish red precipitate, and the solution in the mixed system A is neutral to ensure that pure Fe (OH) is obtained3And Bi (OH)3Precipitate without NO3 —The BiFeO can be obtained after the hydrothermal reaction3NaOH and H2O mixed liquor, washing until the washed washing liquor is neutral, and drying BiFeO3Obtaining flower-shaped BiFeO with the grain diameter of about 1 mu m3And (3) powder. The invention successfully prepares BiFeO with a flower-shaped structure3Powder, wherein the powder is formed by piling up pieces into flowers.
Furthermore, the filling degree and the heating rate of the precursor liquid in the reaction kettle are controlled to reduce the influence of the outside on the reaction process, so that the preparation process has good repeatability.
Drawings
FIG. 1 shows flower-like BiFeO prepared in example 1 of the present invention3XRD pattern of the powder.
FIG. 2 shows flower-shaped BiFeO prepared in example 1 of the present invention3SEM image of powder.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Compared with a high-temperature solid phase method, a sol-gel method and a chemical coprecipitation method, the hydrothermal synthesis method adopted by the invention can be carried out at a lower temperature, and the BiFeO obtained3The powder has good crystallization and dispersion characteristics, large specific surface area and surface activityObtaining pure phase BiFeO3And (3) powder.
Example 1
Method for preparing flower-shaped BiFeO by hydrothermal method3The method for preparing the powder comprises the following steps,
step 1, preparing a solution:
fe (NO) is weighed according to the molar ratio of 1:1.053)3·9H2O and Bi (NO)3)3·5H2O, dissolved in 5mL of concentrated HNO3To obtain Fe3+A mother salt solution with a concentration of 0.15mol/L, wherein the mother salt solution is referred to as containing Fe (NO)3)3·9H2O、Bi(NO3)3·5H2O and concentrated HNO3The mixed solution of (1);
step 2, dropwise adding an NaOH solution into the mother salt solution while stirring at the titration speed of 1 mL/min until the pH value is 12 to obtain a brownish red precipitate, continuously stirring for 30min, and standing for 2h to obtain a mixed system A containing the brownish red precipitate;
and 3, repeatedly washing the brownish red precipitate in the mixed system A obtained in the step 2 by using deionized water to enable a washing solution in the mixed system A to be neutral, and removing a supernatant by adopting a filtering mode to obtain the BiFeO prepared by the hydrothermal method3Required precursor powder;
step 4, dropwise adding NaOH solution serving as a mineralizer into the precursor powder while stirring until the pH value of the solution is 12, transferring the solution into a reaction kettle, wherein the filling rate is 80%, the heating rate is 1 ℃/min, the reaction temperature is 200 ℃, and the reaction time is 12 hours;
step 5, taking out the solution after the reaction is finished, washing the product for 4 times by using deionized water until the washed washing liquid is neutral, standing for 2 hours, washing for 2 times by using absolute ethyl alcohol, and drying the product for 15 hours at 50 ℃ to obtain the BiFeO of the rhombohedral crystal system3The powder has a crystal structure of R3C. BiFeO prepared in this example3The average particle size of the powder is 1 to 1.5 μm. The XRD pattern is shown in figure 1, from which it can be seen that BiFeO is prepared3The powder is pure rhombohedral system without other impurity phase. The SEM picture is shown in FIG. 2, from which it can be seen that BiFeO was produced3The powder is flower-shaped, and the average particle size is 1-1.5 mu m.
Example 2
Method for preparing flower-shaped BiFeO by hydrothermal method3The method for preparing the powder comprises the following steps,
step 1, preparing a solution;
fe (NO) is weighed according to the molar ratio of 1:1.023)3·9H2O and Bi (NO)3)3·5H2O, dissolved in 24mL of concentrated HNO3To obtain Fe3+Mother salt solution with the concentration of 0.13 mol/L;
step 2, dropwise adding an NaOH solution into the mother salt solution while stirring at the titration speed of 1.7 mL/min until the pH value is 12 to obtain a brownish red precipitate, continuously stirring for 30min, and standing for 2h to obtain a mixed system A containing the brownish red precipitate;
and 3, repeatedly washing the brownish red precipitate in the mixed system A obtained in the step 2 by using deionized water to enable a washing solution in the mixed system A to be neutral, and removing a supernatant by adopting a filtering mode to obtain the BiFeO prepared by the hydrothermal method3Required precursor powder;
step 4, dropwise adding NaOH solution serving as a mineralizer into the precursor powder while stirring until the pH value of the solution is 12, transferring the solution into a reaction kettle, wherein the filling rate is 80%, the heating rate is 1 ℃/min, the reaction temperature is 180 ℃, and the reaction time is 8 hours;
step 5, taking out the solution after the reaction is finished, washing the product for 4 times by using deionized water until the washed washing liquid is neutral, standing for 2 hours, washing for 2 times by using absolute ethyl alcohol, and drying the product for 15 hours at 60 ℃ to obtain BiFeO3Powder, BiFeO produced3The average particle size of the powder is 1.5 to 2 μm.
Example 3
Method for preparing flower-shaped BiFeO by hydrothermal method3The method for preparing the powder comprises the following steps,
step 1, preparing a solution;
weighing Fe (NO) according to the molar ratio of 1:13)3·9H2O and Bi (NO)3)3·5H2O, dissolved in18mL of concentrated HNO3To obtain Fe3+Mother salt solution with the concentration of 0.14 mol/L;
step 2, dropwise adding a NaOH solution into the mother salt solution while stirring at the titration speed of 1.2 mL/min until the pH value is 11 to obtain a brownish red precipitate, continuously stirring for 40min, and standing for 1h to obtain a mixed system A containing the brownish red precipitate;
and 3, repeatedly washing the brownish red precipitate in the mixed system A obtained in the step 2 by using deionized water to enable a washing solution in the mixed system A to be neutral, and removing a supernatant by adopting a filtering mode to obtain the BiFeO prepared by the hydrothermal method3Required precursor powder;
step 4, dropwise adding NaOH solution serving as a mineralizer into the precursor powder while stirring until the pH value of the solution is 12.5, transferring the solution into a reaction kettle, wherein the filling rate is 75%, the heating rate is 1.5 ℃/min, the reaction temperature is 185 ℃, and the reaction time is 10 hours;
step 5, taking out the solution after the reaction is finished, washing the product with deionized water for 5 times until the washed washing liquid is neutral, standing for 3h, washing with absolute ethyl alcohol for 2 times, drying the product at 70 ℃ for 14h to obtain BiFeO3And (3) powder. The prepared BiFeO3The average particle size of the powder is about 2 μm.
Example 4
Method for preparing flower-shaped BiFeO by hydrothermal method3The method for preparing the powder comprises the following steps,
step 1, preparing a solution;
fe (NO) is weighed according to the molar ratio of 1:1.073)3·9H2O and Bi (NO)3)3·5H2O, dissolved in 10mL of concentrated HNO3To obtain Fe3+Mother salt solution with the concentration of 0.16 mol/L;
step 2, dropwise adding an NaOH solution into the mother salt solution while stirring at the titration speed of 1.5 mL/min until the pH value is 11 to obtain a brownish red precipitate, continuously stirring for 50min, and standing for 1h to obtain a mixed system A containing the brownish red precipitate;
step 3, repeatedly washing the brownish red precipitate in the mixed system A obtained in the step 2 by using deionized water to ensure that the mixed system A is mixed with the red precipitateThe washing liquid in the synthesis system A is neutral, and the supernatant is removed in a filtering way to obtain the BiFeO prepared by the hydrothermal method3Required precursor powder;
step 4, dropwise adding NaOH solution serving as a mineralizer into the precursor powder while stirring until the pH value of the solution is 13, transferring the solution into a reaction kettle, wherein the filling rate is 85%, the heating rate is 1.5 ℃/min, the reaction temperature is 190 ℃, and the reaction time is 14 h;
step 5, taking out the solution after the reaction is finished, washing the product with deionized water for 5 times until the washed washing liquid is neutral, standing for 3h, washing with absolute ethyl alcohol for 3 times, drying the product at 80 ℃ for 12h to obtain BiFeO3And (3) powder. The prepared BiFeO3The average particle size of the powder is about 2.5 μm.
Example 5
Method for preparing flower-shaped BiFeO by hydrothermal method3The method for preparing the powder comprises the following steps,
step 1, preparing a solution;
fe (NO) is weighed according to the molar ratio of 1:1.13)3·9H2O and Bi (NO)3)3·5H2O, dissolved in 30mL of concentrated HNO3To obtain Fe3+Mother salt solution with the concentration of 0.17 mol/L;
step 2, dropwise adding an NaOH solution into the mother salt solution while stirring at the titration speed of 2mL/min until the pH value is 13 to obtain a brownish red precipitate, continuously stirring for 60min, and standing for 1h to obtain a mixed system A containing the brownish red precipitate;
and 3, repeatedly washing the brownish red precipitate in the mixed system A obtained in the step 2 by using deionized water to enable a washing solution in the mixed system A to be neutral, and removing a supernatant by adopting a filtering mode to obtain the BiFeO prepared by the hydrothermal method3Required precursor powder;
step 4, dropwise adding NaOH solution serving as a mineralizer into the precursor powder while stirring until the pH value of the solution is 13, transferring the solution into a reaction kettle, wherein the filling rate is 85%, the heating rate is 2 ℃/min, the reaction temperature is 195 ℃, and the reaction time is 16 h;
step 5, taking out after the reaction is finishedWashing the product with deionized water for 5 times until the washed washing liquid is neutral, standing for 4h, washing with anhydrous ethanol for 3 times, and drying the product at 80 ℃ for 13h to obtain BiFeO3And (3) powder. The prepared BiFeO3The average particle size of the powder is about 3 μm.
Claims (2)
1. Method for preparing flower-shaped BiFeO by hydrothermal method3The powder preparation method is characterized by comprising the following steps:
step 1, preparing a solution, and adding Fe (NO) according to a molar ratio of 1 (1.02-1.07)3)3·9H2O and Bi (NO)3)3·5H2Dissolving O in nitric acid to obtain Fe3+Mother salt solution with the concentration of 0.14-0.16 mol/L; the nitric acid is concentrated nitric acid, and the volume of the concentrated nitric acid is 4-30 mL;
step 2, adjusting the pH value of the mother salt solution to 11-13 by a method of dripping NaOH solution while stirring, wherein the titration rate of the NaOH solution is 1-2 mL/min, and obtaining a mixed system A containing a brownish red precipitate;
step 3, washing the brownish red precipitate in the mixed system A until the washing liquid is neutral, and filtering to obtain hydrothermal precursor powder;
step 4, regulating the pH value of the hydrothermal precursor powder to 12-13 by using a NaOH solution to obtain a mixed system B, carrying out hydrothermal reaction on the mixed system B at 180-200 ℃ for 8-16 h, washing the product until the washed washing liquid is neutral, and drying the obtained product to obtain flower-shaped BiFeO3Powder, wherein the powder is formed by piling up pieces into flowers;
after the red brown precipitate is obtained in the step 2, stirring for 30-60 min, and standing for 1-2 h to obtain a mixed system A containing the red brown precipitate;
step 4, transferring the mixed system B into a reaction kettle for hydrothermal reaction, wherein the filling rate of the reaction kettle is 75-85%;
in the step 4, the heating rate of the mixed system B reaching the reaction temperature is 1-2 ℃/min;
after the reaction of the mixed system B in the step 4, washing the product with deionized water for 4-5 times until the washed washing liquid is neutral, washing with absolute ethyl alcohol for 2-3 times, and standing for 2-4 hours to obtain a product;
drying the product obtained in the step 4 at 50-80 ℃ for 12-15 h to obtain flower-shaped BiFeO3Powder;
the filling degree and the heating rate of the precursor liquid in the reaction kettle are controlled to reduce the influence of the outside on the reaction process, so that the preparation process has repeatability.
2. Flower-shaped BiFeO prepared by the method of claim 13And (3) powder.
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| CN106698521A (en) * | 2017-02-27 | 2017-05-24 | 陕西科技大学 | Three-dimensional flower-shaped bismuth ferrite powder and preparation method thereof |
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