CN113860863B - Light Ba 2 Co 2 Fe 12 O 22 Preparation method of porous ferrite absorbent - Google Patents
Light Ba 2 Co 2 Fe 12 O 22 Preparation method of porous ferrite absorbent Download PDFInfo
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Abstract
The invention relates to the field of microwave absorption and discloses light Ba 2 Co 2 Fe 12 O 22 The preparation method of porous ferrite absorbent comprises activating dried yeast powder to obtain yeast cell solution, and adding Ba 2+ ,Co 2+ ,Fe 3+ Sequentially adding salt solution into yeast cell solution, continuously stirring to make metal ions fully adsorbed on yeast cell surface, mineralizing metal ions on yeast cell surface by biomineralization to obtain uniform sol containing yeast solution, heating to remove solvent to obtain dried gel, heat treating dried gel to remove yeast cell to obtain light Ba 2 Co 2 Fe 12 O 22 A ferrite absorbent. The invention takes natural yeast cells as a structural template, adopts a simple sol-gel technology, has simple process, avoids the complicated process and the use of a large amount of solvents, and realizes light Ba 2 Co 2 Fe 12 O 22 The ferrite absorbent is prepared in a low-cost and environment-friendly way.
Description
Technical Field
The invention relates to the technical field of microwave absorption, in particular to light Ba 2 Co 2 Fe 12 O 22 A method for producing a (BCFO) ferrite absorbent.
Background
The ferrite becomes the most common microwave absorbent due to higher magnetic permeability value and low preparation cost, has the remarkable advantages of high absorption efficiency, wide absorption frequency band, thin thickness and the like, and has good application prospect in the field of microwave absorption. However, ferrite has a large specific gravity, which increases the weight of the parts, limiting their wide application in the microwave absorption field. Therefore, the reduction of the specific gravity of the ferrite while ensuring the good wave absorption performance of the ferrite is a key problem to be solved urgently for realizing the wide application of the ferrite in the microwave absorption field.
The preparation of the porous ferrite is an effective way for reducing the specific gravity of the ferrite and improving the wave absorption performance of the ferrite. On one hand, the porous ferrite can reduce the specific gravity of the material, and on the other hand, the porous structure can absorb electromagnetic waves and deflect and scatter the electromagnetic waves, so that the porous ferrite can obviously enhance the wave absorbing performance of the material.
At present, researchers mainly adopt a template method for preparing the porous ferrite. In the method, the preparation of the porous material by using the carbon microspheres as the hard template has the obvious advantages of safe and nontoxic preparation process, simple process, low cost and no need of surface treatment on the template. However, the carbon-based microspheres are easy to crosslink and agglomerate when being used as a template, and the application of the carbon microspheres as the template in the actual synthesis process is limited. Therefore, the selection of a proper template is crucial to the successful preparation of the porous ferrite.
In fact, there are many surprising and impressive structures in nature, such as multilevel ordered organization structures, periodic nanostructures, and these special morphologies also provide special functions to these organisms or materials. The biological material with a special structure is used as a template, which is an effective way for synthesizing controllable and unique morphological structure materials. The research of synthesizing materials with special structures by a biological template method has been reported, but the research of synthesizing porous ferrite by using yeast cells as a template agent has been rarely reported.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides light Ba 2 Co 2 Fe 12 O 22 The preparation method of porous ferrite absorbent uses natural yeast cells as template, barium nitrate, cobalt nitrate and ferric nitrate as barium source, cobalt source and iron source, and adopts biomineralization principle and sol-gel technology to prepare light Ba 2 Co 2 Fe 12 O 22 Porous ferrite absorber for realizing light Ba 2 Co 2 Fe 12 O 22 The porous ferrite absorbent is prepared in a low-cost and environment-friendly manner, the use of a complex process and a large amount of solvents is avoided, the subsequent treatment process is reduced, and the porous ferrite absorbent is economic and environment-friendly.
The technical scheme is as follows: the invention provides a light Ba 2 Co 2 Fe 12 O 22 The preparation method of the porous ferrite absorbent comprises the following steps: s1: activating the dried yeast powder to obtain a yeast cell solution; s2: ba is mixed with 2+ 、Co 2+ And Fe 3+ Adding salt solution into the yeast cell solution in sequence, and stirring continuously to enable Ba to be in the solution 2+ 、Co 2+ And Fe 3+ Sufficiently adsorbed on the surface of yeast cells and made Ba by biomineralization 2+ 、Co 2+ And Fe 3+ Mineralizing the surface of yeast cells to obtain uniform sol containing yeast solution, and then heating to remove the solvent to obtain dry gel; s3: heat treatment to remove yeast cells in the xerogel and obtain light Ba 2 Co 2 Fe 12 O 22 A porous ferrite absorbent.
Preferably, in the S1, the activation conditions of the dry yeast powder are dry yeast (g): anhydrous glucose (g): water (mL) = 3-6: 0.8-1.2: 200-300; carrying out water bath for 30 min at the temperature of 35-40 ℃. Preferably dry yeast (g): anhydrous glucose (g): water (mL) =5:1:250, water bath 30 min at 37 ℃.
Preferably, in the S2, the concentration of the yeast cell solution is 10 g.L -1 ~30g· L -1 . Preferably 10 g.L -1 , 20g·L -1 , 30g·L -1 。
Preferably, in the S2, the Ba 2+ 、Co 2+ 、Fe 3+ The salt solution is nitrate, and barium nitrate, cobalt nitrate and ferric nitrate are added according to a stoichiometric ratio, wherein the mass ratio of the barium nitrate to the dried yeast powder is 1.5-5.5, and preferably 1.74, 2.61 and 5.2.
Preferably, in the S2, the Ba 2+ 、Co 2+ 、Fe 3+ The mineralization time on the surface of the yeast cell is 8-16 h.
Preferably, in the step S2, the heating temperature for heating to remove the solvent to obtain the xerogel is 120-160 ℃, and the heating time is 8-14 h.
Preferably, in the S3, the temperature of the heat treatment is 1000-1100 ℃ and the time is 3-6 h.
The principle and the beneficial effects are as follows:
the preparation principle of the invention is as follows:
firstly, activating dry yeast under certain conditions to obtain yeast cell solution, and then adding Ba with certain concentration 2+ 、Co 2+ And Fe 3+ Sequentially adding salt solution into the yeast solution, stirring, and making metal ion Ba by using electrostatic adsorption principle 2+ 、Co 2+ And Fe 3+ Sufficiently adsorbed on the surface of yeast cells and can make metal ions Ba through biomineralization 2+ 、Co 2+ And Fe 3+ Mineralize on the surface of yeast cell to obtain homogeneous sol containing yeast solution, and then heat at certain temperature to eliminate solvent to obtain dry gel. Heat treating the xerogel at a certain temperature to remove the yeast cell template, thus obtaining the light Ba 2 Co 2 Fe 12 O 22 A porous ferrite absorbent.
To realize light Ba 2 Co 2 Fe 12 O 22 The invention relates to green and environment-friendly preparation of a porous ferrite absorbent. The yeast is a single-cell fungus, the cell width is about 2-6 mu m, the cell length is about 5-30 mu m, and the cell has the shapes of a sphere, an oval, an ellipse and the like. The yeast cells have special multistage nano-net structure and selfThe assembly mode is provided with a plurality of nano micropores and surface functional regions, and the nano micropores and the surface functional regions contain a large number of hydrophilic groups, the hydrophilic groups play the role of soft templates in the biomineralization process, and the yeast cells play the role of hard templates. And, the yeast cell surface has OH - ，-COO - and-OPO 3 2- Plasma negative ions with a large amount of negative charges on the surface, and inorganic metal salts are often used for synthetic ferrite materials, so that free metal ions (Ba) are generated 2+ 、Co 2+ And Fe 3+ ) The porous ferrite material can be electrostatically adsorbed on the surface of yeast cells and self-assembled on the surface of the yeast cells, and can be obtained through biomineralization and calcination treatment.
Compared with the prior art for preparing the porous ferrite absorbent, the porous ferrite absorbent has the following advantages:
1) the yeast cells are used as the biological template, the preparation process is green and environment-friendly, the agglomeration problem caused by the carbon microspheres used as the template is avoided, and the porous ferrite absorbent prepared by the method has uniform pore distribution and controllable pore diameter, and can effectively regulate and control the microstructure of the porous ferrite.
2) The preparation method adopts a sol-gel method, the solvent is water, the use of harmful solvents is not involved, the preparation method is safe and environment-friendly, the preparation process is simple and easy to operate, and the green and environment-friendly preparation of the porous ferrite absorbent can be realized.
3) The yeast cells which are natural and uniformly dispersed are used for replacing an expensive and easily-agglomerated synthetic carbon microsphere template, so that the low-cost, green and environment-friendly and structure-controllable preparation of the porous ferrite absorbent is realized.
4）Ba 2+ 、Co 2+ And Fe 3+ Is adsorbed on the surface of yeast cells by the electrostatic adsorption principle and enables Ba to be adsorbed on the surface of yeast cells by the biomineralization principle 2+ 、Co 2+ And Fe 3+ The surface of the yeast cell is mineralized and crystallized to generate a precursor solution of the ferrite, which is more beneficial to the smooth proceeding of the heat treatment process and effectively regulates and controls the structure of the porous ferrite.
5) The invention adopts a sol-gel technology, the technology is simple and easy to operate, does not relate to the use of organic solvents, reduces the subsequent treatment process, and is economic and environment-friendly.
Drawings
FIG. 1 shows that (a) the concentration of the yeast-free template (BCFO) and (b) the concentration of the yeast cell solution were 10 g.L -1 (BCFO-10), (c) Yeast cell solution concentration of 20 g.L -1 (BCFO-20), (d) Yeast cell solution concentration of 30 g.L -1 (BCFO-30) XRD pattern of sample after heat treatment of porous ferrite at 1100 deg.C;
FIG. 2 is SEM photographs of samples of porous ferrites (a) BCFO, (b) BCFO-10, (c) BCFO-20, (d) BCFO-30 after heat treatment at a temperature of 1100 ℃;
FIG. 3 is a real part (a) of dielectric constant of a sample after heat treatment of BCFO, BCFO-10 porous ferrite at a temperature of 1100 ℃; an imaginary part (b); a real permeability part (c); an imaginary part (d).
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Embodiment 1:
passing 0.5g of dry yeast powder through dry yeast (g): anhydrous glucose (g): water (mL) =5:1:250, water bath at 37 deg.C for 30 min activation, centrifuging to remove glucose, washing with water for 3 times, adding into 50mL deionized water to obtain a concentration of 10 g.L -1 The yeast cell solution of (4); then 2.61 g of barium nitrate, 2.91 g of cobalt nitrate, 24.24 g of ferric nitrate and 23.04 g of complexing agent citric acid are sequentially added into the yeast cell solution, and stirring is continuously carried out to ensure that metal ions Ba 2+ 、Co 2+ And Fe 3+ Sufficiently adsorbed on the surface of yeast cells and can make metal ions Ba through biomineralization 2+ 、Co 2+ And Fe 3+ Mineralizing the surface of the yeast cells for 12 hours to obtain uniform sol containing yeast cell solution; then heating at 140 ℃ for 12h to remove the solvent to obtain xerogel; the dried gel is thermally treated at the temperature of 1100 ℃ for 4h to remove the yeast cell template, and the light Ba is obtained 2 Co 2 Fe 12 O 22 A porous ferrite absorbent.
Embodiment 2:
the present embodimentSubstantially the same as embodiment 1, but different therefrom only in that: 1.0g of dry yeast powder was passed through dry yeast (g): anhydrous glucose (g): water (mL) =5:1:250, water bath at 37 deg.C for 30 min for activation, centrifuging to remove glucose, washing with water for 3 times, adding into 50mL deionized water to obtain 20 g.L -1 The yeast cell solution of (1).
Otherwise, this embodiment is identical to embodiment 1, and will not be described herein.
Embodiment 3:
this embodiment is substantially the same as embodiment 1, and differs only in that: 1.5g of dry yeast powder was passed through dry yeast (g): anhydrous glucose (g): water (mL) =5:1:250, water bath at 37 deg.C for 30 min for activation, centrifuging to remove glucose, washing with water for 3 times, adding into 50mL deionized water to obtain a concentration of 30 g.L -1 The yeast cell solution of (1).
Otherwise, this embodiment is identical to embodiment 1, and will not be described herein. .
Embodiment 4:
50mL of deionized water is taken to replace yeast cell solution, then 2.61 g of barium nitrate, 2.91 g of cobalt nitrate, 24.24 g of ferric nitrate and 23.04 g of complexing agent citric acid are sequentially added into the deionized water, and the mixture is continuously stirred to ensure that metal ions Ba are generated 2+ 、Co 2+ And Fe 3+ Fully dissolving for 12 hours to obtain uniform sol; then heating at 140 ℃ for 12h to remove the solvent to obtain xerogel; heat treating the xerogel at 1100 deg.c for 4 hr to obtain Ba 2 Co 2 Fe 12 O 22 A ferrite absorbent. Ba produced in embodiments 1 to 4 described above 2 Co 2 Fe 12 O 22 The XRD pattern of the ferrite absorbent is shown in figure 1. The XRD pattern of the product is consistent with the diffraction peak of the XRD pattern (PDF-no-44-0206) of the standard sample, which indicates that the synthesized product is Ba in the above embodiments 2 Co 2 Fe 12 O 22 A ferrite.
Ba produced in embodiments 1 to 4 described above 2 Co 2 Fe 12 O 22 The SEM photograph of the ferrite adsorbent is shown in FIG. 2, and shows that yeast is usedThe sample synthesized by the template has a porous structure, and the structure distribution of the pores is relatively uniform, which indicates that the porous Ba can be successfully synthesized by adopting the yeast cells as the template 2 Co 2 Fe 12 O 22 A ferrite absorbent.
Ba prepared in embodiments 1 and 4 above 2 Co 2 Fe 12 O 22 The electromagnetic parameters of the ferrite absorber are plotted against frequency (8.2-12.4 GHz) as shown in FIG. 3, showing porous Ba 2 Co 2 Fe 12 O 22 The real part and the imaginary part of the dielectric constant of the ferrite (BCFO-10) product are reduced compared with the dielectric constant of the product (BCFO) synthesized without the yeast cell template, the real part of the magnetic permeability is slightly reduced relative to the real part of the magnetic permeability of the BCFO sample, but the imaginary part of the magnetic permeability of the product BCFO-10 is greatly improved compared with the BCFO, which is very beneficial to improving the magnetic loss of the BCFO-10. At the same time, the reduction of the dielectric constant of BCFO-10 contributes to an increase in the level of impedance matching of the product. Overall, the variation of the electromagnetic parameters of the porous BCFO-10 contributes to the improvement of the wave absorption performance thereof.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (3)
1. Light Ba 2 Co 2 Fe 12 O 22 The preparation method of the porous ferrite absorbent is characterized by comprising the following steps:
s1: activating the dried yeast powder to obtain a yeast cell solution;
the activation conditions of the dry yeast powder are as follows: anhydrous glucose: water = 3-6 g, 0.8-1.2 g, 200-300 mL; carrying out water bath for 30 min at 35-40 ℃;
s2: mix Ba with 2+ 、Co 2+ And Fe 3+ Adding salt solution into the yeast cell solution in sequence, and stirring continuously to enable Ba to be in the solution 2+ 、Co 2+ And Fe 3+ Sufficiently adsorbed on the surface of yeast cells and made Ba by biomineralization 2+ 、Co 2+ And Fe 3+ Mineralizing the surface of the yeast cell to obtain a uniform sol containing a yeast cell solution, and then heating to remove the solvent to obtain dry gel;
said Ba 2+ 、Co 2+ 、Fe 3+ The salt solution is nitrate, and barium nitrate, cobalt nitrate and ferric nitrate are added according to a stoichiometric ratio, wherein the mass ratio of the barium nitrate to the dried yeast powder is 1.5-5.5;
said Ba 2+ 、Co 2+ 、Fe 3+ The mineralization time on the surface of the yeast cell is 8-16 h;
s3: heat treatment to remove yeast cells in the xerogel to obtain light Ba 2 Co 2 Fe 12 O 22 A porous ferrite absorbent;
the temperature of the heat treatment is 1000-1100 ℃, and the time is 3-6 h.
2. Light weight Ba of claim 1 2 Co 2 Fe 12 O 22 A method for producing a porous ferrite absorbent, characterized in that the concentration of a yeast cell solution in S2 is 10 g.L -1 ~30g· L -1 。
3. Light weight Ba of claim 1 2 Co 2 Fe 12 O 22 The preparation method of the porous ferrite absorbent is characterized in that in S2, the heating temperature for heating to remove the solvent to obtain the xerogel is 120-160 ℃, and the heating time is 8-14 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674823A (en) * | 2012-05-02 | 2012-09-19 | 中国地质大学（武汉） | Hexagonal crystal system Y-type ferrite electromagnetic material and preparation method thereof |
| CN103449537A (en) * | 2013-08-19 | 2013-12-18 | 长安大学 | Preparation method of nickel molybdate powder material |
| CN109336589A (en) * | 2018-11-02 | 2019-02-15 | 山东科技大学 | A kind of method that microorganism foaming prepares hierarchical porous structure aluminum titanate-mullite ceramics |
| CN109768256A (en) * | 2019-01-18 | 2019-05-17 | 兰州理工大学 | It is a kind of to prepare uniformly carbon-coated LiFePO with saccharomycete4The method of nanocomposite |
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| WO2005023524A2 (en) * | 2003-08-29 | 2005-03-17 | Z Corporation | Absorbent fillers for three-dimensional printing |
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|---|---|---|---|---|
| CN102674823A (en) * | 2012-05-02 | 2012-09-19 | 中国地质大学（武汉） | Hexagonal crystal system Y-type ferrite electromagnetic material and preparation method thereof |
| CN103449537A (en) * | 2013-08-19 | 2013-12-18 | 长安大学 | Preparation method of nickel molybdate powder material |
| CN109336589A (en) * | 2018-11-02 | 2019-02-15 | 山东科技大学 | A kind of method that microorganism foaming prepares hierarchical porous structure aluminum titanate-mullite ceramics |
| CN109768256A (en) * | 2019-01-18 | 2019-05-17 | 兰州理工大学 | It is a kind of to prepare uniformly carbon-coated LiFePO with saccharomycete4The method of nanocomposite |
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| Title |
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| The effect of heat treatment temperature on the microstructure and magnetic properties of Ba2Co2Fe12O22 (Co2Y) prepared by sol–gel method;Nimai Chand Pramanik 等;《materials letters》;20060217;第2718-2722页 * |
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