CN112408498A - Spinel type ferrite CoFe2O4Hydrothermal preparation method of nano powder - Google Patents
Spinel type ferrite CoFe2O4Hydrothermal preparation method of nano powder Download PDFInfo
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- CN112408498A CN112408498A CN202011355616.2A CN202011355616A CN112408498A CN 112408498 A CN112408498 A CN 112408498A CN 202011355616 A CN202011355616 A CN 202011355616A CN 112408498 A CN112408498 A CN 112408498A
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Abstract
The application discloses a spinel type ferrite CoFe2O4A hydrothermal preparation method of nano powder. The method comprises the following steps: (1) dissolving cobalt salt and ferric salt in deionized water to prepare a solution; (2) adding ethanolamine dropwise into the solution prepared in the step (1) while stirring to obtain a precipitate; (3) mixing and stirring the precipitate prepared in the step (1), sodium tartrate, glycerol, diethylene glycol and deionized water; (4) adding epoxidized soybean oil and guar gum into the obtained product in the step (3), and fully stirring; (5) carrying out hydrothermal reaction on the product obtained in the step (4) at the temperature of 160-175 ℃ for 30-35 minutes. The hydrothermal preparation method is simple, convenient and quick to operate, and the prepared nano powder is small in size fluctuation, less in aggregation, high in crystallization degree, excellent in crystal form and good in wave absorbing performance.
Description
Technical Field
The application relates to the field of hydrothermal synthesis, in particular to spinel type ferrite CoFe2O4A hydrothermal preparation method of nano powder.
Background
Ferrite, also known as magnetic ceramic, is a composite oxide magnetic material composed of iron, oxygen and other iron group or rare earth group elements, which is mostly a semiconductor, has a resistivity much higher than that of a general metal magnetic material, and has an advantage of small eddy current loss.
The nano material is characterized in that at least one dimension of the nano material in a three-dimensional space is in a range of 1-100 nanometersThe material in the material has the size in the transition region between the atomic cluster and the macroscopic object, so that the material can show obvious surface effect, small-size effect and macroscopic quantum tunneling effect, and the physical and chemical properties of the material, such as optical, thermal, electrical, magnetic, mechanical properties and the like, are obviously different from those of the material in the macroscopic solid state. As an important direction for the development of the current magnetic nano materials, ferrite nano powder attracts people's extensive attention due to its unique characteristics and advantages, especially CoFe2O4The nano powder is a representative substance of spinel type ferrite, is an important functional material, and shows special electromagnetic properties such as superparamagnetism, giant magnetoresistance effect, magnetic anisotropy, good wave-absorbing performance and the like because the particle size is in a nanometer level. Thus, ferrite CoFe2O4The nano powder is widely applied in the fields of high frequency and microwave technology, such as radar technology, communication technology, space technology, electronic computers and the like.
The ferrite CoFe2O4The preparation method of the nano powder comprises chemical deposition, grinding, high-temperature ignition, hydrothermal synthesis and the like, and the methods have certain problems, such as complex operation, severe reaction conditions, long preparation time, large size fluctuation range of the prepared nano powder, poor crystal form, poor electromagnetic performance and the like.
Therefore, there is a need in the art to develop a spinel ferrite CoFe with simple operation, mild conditions, short time consumption, uniform size of the prepared nanopowder, good crystal form and excellent electromagnetic properties2O4And (3) nano powder.
Disclosure of Invention
[ problem ] to
In view of the disadvantages of the prior art, it is an object of the present application to provide a spinel-type ferrite CoFe2O4A hydrothermal preparation method of nano powder. The hydrothermal preparation method is simple, convenient and quick to operate, and the prepared nano powder is small in size fluctuation, less in aggregation, high in crystallization degree, excellent in crystal form and good in wave absorbing performance.
[ solution ]
To achieve the above objects, there is provided a spinel-type ferrite CoFe according to an embodiment of the present application2O4The hydrothermal preparation method of the nano powder comprises the following steps:
(1) dissolving cobalt salt and ferric salt in deionized water to prepare a solution with the concentration of the cobalt salt being 0.35-0.45 mol/L and the concentration of the ferric salt being 0.70-0.90 mol/L;
(2) adding ethanolamine dropwise into the solution prepared in the step (1) while stirring to obtain a precipitate;
(3) mixing and stirring the precipitate prepared in the step (1), sodium tartrate, glycerol, diethylene glycol and deionized water in the weight ratio of 10 (23-28) to (1.0-1.3) to (0.4-0.7) to (100-120);
(4) adding epoxidized soybean oil and guar gum into the obtained product in the step (3), and fully stirring, wherein the weight ratio of the epoxidized soybean oil and guar gum to the precipitate prepared in the step (1) is (0.06-0.09): 0.12-0.14): 10;
(5) carrying out hydrothermal reaction on the product obtained in the step (4) at the temperature of 160-175 ℃ for 30-35 minutes.
In the present application, the spinel-type ferrite CoFe is prepared by a specific process and adding specific components2O4The nano powder has the advantages of uniform size, small fluctuation range, no agglomeration, excellent crystal form and few defects, and shows excellent wave-absorbing performance.
Further, in the step (1), the molar ratio of the cobalt salt to the iron salt is 1: 2. The molar ratio satisfies CoFe2O4The element ratio (c) can avoid the large influence of redundant Co or Fe.
The cobalt salt may be cobalt chloride or cobalt nitrate.
The iron salt may be ferric chloride or ferric nitrate.
By using the above cobalt and iron salts, the spinel-type ferrite CoFe according to the present application can be better prepared2O4The nano powder has less agglomeration and high crystallization degree.
Further, in the step (2), the usage amount of the ethanolamine may be 7 to 10 times of the molar amount of the iron salt. At this amount, the cobalt and iron salts can be sufficiently precipitated.
In the step (2), the stirring is performed at 120-150 rpm. Under the stirring condition, ethanolamine can be enabled to fully precipitate the cobalt salt and the iron salt.
And (3) centrifugally washing the obtained precipitate for 2-3 times by using deionized water and airing.
Further, in the step (3), the stirring is carried out at 600-700 rpm for 15-20 minutes. Under the stirring condition, the components of the sodium tartrate, the glycerol and the diethylene glycol can be fully mixed and fully contacted with the precipitate, so that the precipitate is activated.
Further, in the step (4), the stirring is performed at 400 to 500rpm for 5 to 7 minutes. Under the stirring condition, the activated precipitate can be fully contacted with the epoxidized soybean oil and the guar gum, and good conditions are created for the next hydrothermal reaction.
Further, in the step (5), the temperature rise rate of the hydrothermal reaction is 7.0-8.0 ℃/min. At this temperature increase rate, the formation of the spinel crystal form can be promoted better.
The cooling rate after the hydrothermal reaction is finished is 2.0-2.5 ℃/min. Under the cooling rate, the spinel crystal form with higher crystallization degree can be maintained, and lattice defects are avoided.
Further, in the step (5), the hydrothermal reaction is performed in a stainless steel reaction kettle provided with a polytetrafluoroethylene lining.
Further, the hydrothermal preparation method according to the present application further includes, after the step (5) above:
(6) and (4) centrifugally cleaning and washing the obtained substance in the step (5) for 2-3 times by using deionized water, and then drying for 5-6 hours in vacuum at 70-80 ℃.
[ advantageous effects ]
In summary, the present application has the following beneficial effects:
hydrothermal preparation method according to the present applicationThe method needs short time, and the prepared spinel type ferrite CoFe2O4The nanometer powder is prepared. The hydrothermal preparation method is simple, convenient and quick to operate, and the prepared nano powder is small in size fluctuation, less in aggregation, high in crystallization degree, excellent in crystal form and good in wave absorbing performance.
Drawings
FIG. 1 shows a spinel-type ferrite CoFe prepared according to example 1 of the present application2O4X-ray diffraction pattern of the nanopowder;
FIG. 2 shows a spinel-type ferrite CoFe prepared according to example 2 of the present application2O4X-ray diffraction pattern of the nanopowder;
FIG. 3 shows a spinel-type ferrite CoFe prepared according to example 3 of the present application2O4X-ray diffraction pattern of the nanopowder;
FIG. 4 shows a spinel-type ferrite CoFe prepared according to example 4 of the present application2O4X-ray diffraction pattern of the nanopowder;
FIG. 5 shows ferrite CoFe prepared according to comparative example 1 of the present application2O4An X-ray diffraction pattern of the powder;
FIG. 6 shows spinel-type ferrite CoFe prepared according to examples 1 to 4(A to D) of the present application2O4Transmission electron microscopy of the nanopowder; and
FIG. 7 shows ferrite CoFe prepared according to comparative example 1 of the present application2O4Transmission electron microscopy of the powder.
Detailed Description
In order that those skilled in the art can more clearly understand the present application, the present application will be described in further detail with reference to the following examples, but it should be understood that the following examples are only preferred embodiments of the present application, and the scope of the present application as claimed is not limited thereto.
Sources of materials
Cobalt nitrate (Co (NO)3)2·6H2O), ferric nitrate (Fe (NO)3)3) Cobalt chloride (C)oCl2·6(H2O)) and ferric chloride (FeCl)3) From alfa aesar (china) chemical co.
Instrumentation and equipment
Powder X-ray diffractometer model D/max2550VL/PC manufactured by Japan science;
a high-resolution transmission electron microscope, model JEOL JEM-2100F, manufactured by JEOL, Japan Electron Co.
< example >
Example 1
The following hydrothermal preparation method according to the present application was used to prepare spinel-type ferrite CoFe2O4Nano powder:
(1) 0.35mol (101.87g) of cobalt nitrate (Co (NO)3)2·6H2O) and 0.70mol (169.30g) of iron nitrate (Fe (NO)3)3) Dissolving the mixture in deionized water to prepare a solution with the concentration of cobalt nitrate being 0.35mol/L and the concentration of ferric nitrate being 0.70 mol/L;
(2) adding 420g of ethanolamine dropwise into the solution prepared in the step (1) and stirring at 150rpm to obtain 107.5g of precipitate, centrifugally washing the obtained precipitate with deionized water for 2 times and airing;
(3) mixing 100g of the precipitate obtained in the step (1), 230g of sodium tartrate, 13g of glycerin, 5.0g of diethylene glycol and 1000g of deionized water, and stirring at 700rpm for 15 minutes;
(4) adding 6.0g of epoxidized soybean oil and 14g of guar gum to the resultant of the step (3), and sufficiently stirring at 400rpm for 7 minutes;
(5) adding the obtained substance in the step (4) into a stainless steel reaction kettle provided with a polytetrafluoroethylene lining, heating to 175 ℃ at the heating rate of 7.0 ℃/min, carrying out hydrothermal reaction for 30 minutes at the temperature, and then cooling to room temperature at the cooling rate of 2.0 ℃/min;
(6) and (3) centrifugally washing the obtained substance in the step (5) with deionized water for 3 times, and then drying the substance in vacuum at 80 ℃ for 5 hours.
Thus, spinel type ferrite CoFe is obtained2O4And (3) nano powder.
Example 2
The following hydrothermal preparation method according to the present application was used to prepare spinel-type ferrite CoFe2O4Nano powder:
(1) 0.45mol (130.97g) of cobalt nitrate (Co (NO)3)2·6H2O) and 0.90mol (145.98g) of iron chloride (FeCl)3) Dissolving the mixture in deionized water to prepare a solution with the concentration of cobalt nitrate being 0.45mol/L and the concentration of ferric chloride being 0.90 mol/L;
(2) adding 420g of ethanolamine dropwise into the solution prepared in the step (1), stirring at 120rpm to obtain 138.0g of precipitate, centrifugally washing the precipitate with deionized water for 3 times, and airing;
(3) mixing 100g of the precipitate obtained in the step (1), 280g of sodium tartrate, 12g of glycerol, 4.0g of diethylene glycol and 1200g of deionized water, and stirring at 600rpm for 20 minutes;
(4) adding 7.5g of epoxidized soybean oil and 13g of guar gum to the resultant of the step (3), and sufficiently stirring at 500rpm for 5 minutes;
(5) adding the obtained substance in the step (4) into a stainless steel reaction kettle provided with a polytetrafluoroethylene lining, heating to 160 ℃ at the heating rate of 8.0 ℃/min, carrying out hydrothermal reaction for 35 minutes at the temperature, and then cooling to room temperature at the cooling rate of 2.5 ℃/min;
(6) and (3) centrifugally washing the obtained substance in the step (5) with deionized water for 3 times, and then drying the substance in vacuum at 70 ℃ for 6 hours.
Thus, spinel type ferrite CoFe is obtained2O4And (3) nano powder.
Example 3
The following hydrothermal preparation method according to the present application was used to prepare spinel-type ferrite CoFe2O4Nano powder:
(1) 0.40mol (95.17g) of cobalt chloride (CoCl)2·6(H2O)) and 0.80mol (193.49g) of iron nitrate (Fe (NO))3)3) Dissolving in deionized water to obtain cobalt chloride with concentration of 0.40mol/L solution with ferric nitrate concentration of 0.80 mol/L;
(2) dropwise adding 400g of ethanolamine into the solution prepared in the step (1), stirring at 140rpm to obtain 122.7g of precipitate, centrifugally washing the precipitate with deionized water for 3 times, and airing;
(3) mixing 100g of the precipitate obtained in step (1), 250g of sodium tartrate, 10g of glycerol, 7.0g of diethylene glycol and 1100g of deionized water, and stirring at 650rpm for 17 minutes;
(4) adding 9.0g of epoxidized soybean oil and 12g of guar gum to the resultant of the step (3), and sufficiently stirring at 450rpm for 6 minutes;
(5) adding the obtained substance in the step (4) into a stainless steel reaction kettle provided with a polytetrafluoroethylene lining, heating to 165 ℃ at the heating rate of 7.0 ℃/min, carrying out hydrothermal reaction for 30 minutes at the temperature, and then cooling to room temperature at the cooling rate of 2.0 ℃/min;
(6) and (3) centrifugally washing the obtained substance in the step (5) with deionized water for 3 times, and then drying the substance in vacuum at 70 ℃ for 5 hours.
Thus, spinel type ferrite CoFe is obtained2O4And (3) nano powder.
Example 4
The following hydrothermal preparation method according to the present application was used to prepare spinel-type ferrite CoFe2O4Nano powder:
(1) 0.40mol (95.17g) of cobalt chloride (CoCl)2·6(H2O)) and 0.80mol (129.76g) of iron chloride (FeCl)3) Dissolving in deionized water to obtain a solution with the concentration of cobalt chloride of 0.40mol/L and the concentration of ferric chloride of 0.80 mol/L;
(2) dropwise adding 450g of ethanolamine into the solution prepared in the step (1), stirring at 130rpm to obtain 122.5g of precipitate, centrifugally washing the obtained precipitate with deionized water for 2 times, and airing;
(3) mixing 100g of the precipitate obtained in the step (1), 260g of sodium tartrate, 11g of glycerin, 6.0g of diethylene glycol and 1200g of deionized water, and stirring at 700rpm for 17 minutes;
(4) adding 6.0g of epoxidized soybean oil and 12g of guar gum to the resultant of the step (3), and sufficiently stirring at 450rpm for 5 minutes;
(5) adding the obtained substance in the step (4) into a stainless steel reaction kettle provided with a polytetrafluoroethylene lining, heating to 165 ℃ at the heating rate of 7.0 ℃/min, carrying out hydrothermal reaction for 35 minutes at the temperature, and then cooling to room temperature at the cooling rate of 2.0 ℃/min;
(6) the resultant of step (5) was washed 2 times with deionized water by centrifugal washing, followed by vacuum drying at 75 ℃ for 5.5 hours.
Thus, spinel type ferrite CoFe is obtained2O4And (3) nano powder.
Comparative example 1
Ferrite CoFe was performed in the same manner as in example 1, except that steps (3) and (4) were not employed2O4And (3) preparing powder.
< test examples >
(1)Diffraction by X-ray
Determination of the spinel-type ferrite CoFe obtained in examples 1 to 4 by means of X-ray diffractometer model D/max2550VL/PC2O4Nanopowder and ferrite CoFe prepared in comparative example 12O4The XRD patterns of the powders are shown in FIGS. 1 to 5.
As can be seen from FIGS. 1 to 4, spinel-type ferrite CoFe prepared according to examples 1 to 4 of the present application2O4The nanometer powder has good crystal form and clear and obvious diffraction peak. In contrast, ferrite CoFe of comparative example 1 shown in FIG. 52O4The diffraction peak of the powder is obviously widened and cannot be compared with an XRD standard card, which shows that the crystallization degree of the hydrothermal product is obviously poor.
(2)Transmission Electron Microscope (TEM)
Determination of spinel-type ferrite CoFe obtained in examples 1 to 4 by JEOL JEM-2100F type high-resolution transmission electron microscope2O4Nanopowder and ferrite CoFe prepared in comparative example 12O4TEM images of the powder, the results are shown in FIGS. 6 and 7.
As can be seen from FIG. 6, spinel-type ferrite CoFe prepared according to examples 1 to 4 of the present application2O4The particle size of the nano powder (respectively corresponding to (A) to (D)) is basically 20-30 nm, the size is uniform and regular, and the agglomeration phenomenon does not occur, thus proving that the nano powder with good properties is prepared. In contrast, ferrite CoFe of comparative example 1 shown in FIG. 72O4The size of the powder is changed greatly, the particle size is 10-50 nm, the uniformity is poor, irregular fragments exist, and the agglomeration phenomenon is obvious.
(3)Wave absorbing property
50g each of the spinel-type ferrite CoFe obtained in examples 1 to 42O4Nanopowder and ferrite CoFe prepared in comparative example 12O4The powder was mixed with 40g of bisphenol A epoxy resin, respectively, and dispersed by stirring at 1200rpm for 40 minutes, then 10g of a low molecular amine curing agent was added, followed by aging by stirring for 30 minutes, then 7g of a xylene solvent and 0.2g of a film-forming aid were added, and the resulting mixtures were coated on an aluminum plate of 180mm × 180mm in thickness, respectively, and then baked at 50 ℃ for 1 hour, and then cooled to room temperature. The areal density (kg/m) of each sample in the range of 300MHz to 30GHz was then determined2) And the wave-absorbing bandwidth (GHz) and the wave-absorbing peak value (dB) of the Reflection Loss (RL) below-20 dB.
The test results of the above-described respective wave absorption properties are shown in the following table 1:
[ Table 1]
| Areal density (kg/m)2) | Wave-absorbing bandwidth (GHz) | Peak wave absorption (dB) | |
| Example 1 | 1.1 | 3.32 | -62.9 |
| Example 2 | 1.2 | 3.66 | -56.3 |
| Example 3 | 1.0 | 3.51 | -66.8 |
| Example 4 | 1.1 | 3.47 | -51.8 |
| Comparative example 1 | 1.9 | 1.58 | -34.1 |
As can be seen from the above Table 1, spinel-type ferrite CoFe prepared according to examples 1 to 4 of the present application2O4The nanopowder exhibited very good wave absorption properties, while the ferrite CoFe of comparative example 12O4The wave-absorbing performance of the powder is obviously poor.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. Spinel type ferrite CoFe2O4The hydrothermal preparation method of the nano powder is characterized by comprising the following steps:
(1) dissolving cobalt salt and ferric salt in deionized water to prepare a solution with the concentration of the cobalt salt being 0.35-0.45 mol/L and the concentration of the ferric salt being 0.70-0.90 mol/L;
(2) adding ethanolamine dropwise into the solution prepared in the step (1) while stirring to obtain a precipitate;
(3) mixing and stirring the precipitate prepared in the step (1), sodium tartrate, glycerol, diethylene glycol and deionized water in the weight ratio of 10 (23-28) to (1.0-1.3) to (0.4-0.7) to (100-120);
(4) adding epoxidized soybean oil and guar gum into the obtained product in the step (3), and fully stirring, wherein the weight ratio of the epoxidized soybean oil and guar gum to the precipitate prepared in the step (1) is (0.06-0.09): 0.12-0.14): 10;
(5) carrying out hydrothermal reaction on the product obtained in the step (4) at the temperature of 160-175 ℃ for 30-35 minutes.
2. The hydrothermal preparation method according to claim 1, wherein in the step (1), the molar ratio of the cobalt salt to the iron salt is 1: 2.
3. The hydrothermal preparation method of claim 1, wherein the cobalt salt is cobalt chloride or cobalt nitrate; the iron salt is ferric chloride or ferric nitrate.
4. The hydrothermal preparation method according to claim 1, wherein in the step (2), the amount of the ethanolamine is 7 to 10 times of the molar amount of the iron salt, and the stirring is performed at 120 to 150 rpm.
5. The hydrothermal preparation method according to claim 1, wherein the step (2) further comprises washing the obtained precipitate with deionized water by centrifugation 2-3 times and drying.
6. The hydrothermal preparation method according to claim 1, wherein in the step (3), the stirring is performed at 600 to 700rpm for 15 to 20 minutes.
7. The hydrothermal preparation method according to claim 1, wherein in the step (4), the stirring is performed at 400 to 500rpm for 5 to 7 minutes.
8. The hydrothermal preparation method according to claim 1, wherein in the step (5), the temperature increase rate of the hydrothermal reaction is 7.0-8.0 ℃/min, and the temperature decrease rate after the completion of the hydrothermal reaction is 2.0-2.5 ℃/min.
9. The hydrothermal preparation method of claim 1, wherein in step (5), the hydrothermal reaction is performed in a stainless steel reaction kettle provided with a polytetrafluoroethylene lining.
10. The hydrothermal preparation method of claim 1, further comprising, after the step (5):
(6) and (4) centrifugally cleaning and washing the obtained substance in the step (5) for 2-3 times by using deionized water, and then drying for 5-6 hours in vacuum at 70-80 ℃.
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