CN111785471B - Amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, preparation method thereof and magnetic core - Google Patents
Amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, preparation method thereof and magnetic core Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/38—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites amorphous, e.g. amorphous oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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Abstract
The invention discloses an amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, a preparation method and a magnetic core, wherein the composite material is prepared from nanocrystalline Fe 3 O 4 And amorphous SiO 2 The nano particles are mutually and uniformly dispersed, and the particle diameters of the nano particles and the nano particles are less than 5nm. The composite material is prepared by adopting a low-temperature water bath method in one step: weighing a certain amount of FeCl 2 Dissolving sodium acetate and ethyl orthosilicate in a mixed solvent of DMF and water, magnetically stirring in a water bath kettle at the temperature of 80-90 ℃, after reacting for 2-4 hours, sequentially adopting water and alcohol to carry out magnetic separation and cleaning, and drying at room temperature to obtain the composite material. The magnetic core pressed by the amorphous nanocrystalline composite material can be used for inhibiting and absorbing high-frequency interference signals.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to an amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, a preparation method thereof and a magnetic core using the same.
Background
As the frequency of use of electronic products increases, the frequency of interference signals in electronic circuits also increases. The anti-electromagnetic interference magnetic ring on the current market mainly comprises ferrite materials. The suppression frequency range varies with different ferrite materials. Wherein the manganese zinc ferrite is mainly suitable for low frequency below 30 MHz. While nickel zinc ferrites may be suitable for higher frequencies, such as 25MHz to 200MHz. However, as the frequency of devices and systems increases, the current manganese zinc ferrite and nickel zinc ferrite cannot meet the frequency requirement. Therefore, it is necessary to develop a magnetic core material capable of suppressing an interference signal of 200MHz or more. The use frequency of the material is improved, on one hand, the structure of the material is reformed, on the other hand, the particle size of the magnetic material is reduced, and the internal structure is changed by adopting methods such as composite materials and the like.
The composite material is added with insulating materials such as silicon dioxide and the like, so that the resistivity can be improved, the eddy current loss can be effectively reduced, and the use frequency of the magnetic material can be improved. However, in the current preparation method, nano silica powder is added into a soft magnetic material, then ball milling is carried out, so that the silica and the magnetic material are uniformly mixed, and finally, the composite material is obtained after high-temperature heating. However, the preparation method has complex process and long time, and the uniformity of the material can not be ensured. Meanwhile, the crystal grains are enlarged in the high-temperature treatment process, the high-frequency property of the material is not facilitated, and the social energy loss is increased by the high-temperature sintering treatment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses an amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, a preparation method and a magnetic core 3 O 4 And amorphous SiO 2 The nano particles are mutually and uniformly dispersed, and the particle diameters of the nano particles and the nano particles are less than 5nm. The magnetic core pressed by the composite material has high impedance above 200MHz and low impedance in a frequency band lower than 2 MHz.
In order to realize the composite material, the technical scheme of the invention is as follows:
an amorphous nanocrystalline high-frequency anti-interference magnetic core composite material is prepared from nanocrystalline Fe 3 O 4 And amorphous SiO 2 The nano particles are mutually and uniformly dispersed, and the particle diameters of the nano particles and the nano particles are less than 5nm. Due to the nanocrystalline Fe in the composite material 3 O 4 Has good crystallinity and the composite material has good paramagnetic property.
As a further improvement scheme, the composite material is prepared by adopting a low-temperature water bath method.
The invention also discloses a preparation method of the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material, which comprises the following steps:
step S1, measuring dimethyl formamide DMF and distilled water with a volume ratio of 8, and mixing to obtain a mixed solvent;
step S2, feCl is added 2 ·4H 2 O, ethyl orthosilicate and sodium acetate, stirring for 10 minutes at normal temperature until the O, the ethyl orthosilicate and the sodium acetate are fully dissolved and uniformly mixed to obtain a mixed solution, wherein FeCl 2 ·4H 2 The concentration of O relative to the mixed solvent is 10-15 mg/mL, the volume ratio of the ethyl orthosilicate to the mixed solvent is 0.001;
s3, stirring the mixed solution in a constant-temperature water bath for 2-4 hours for full reaction;
and S4, taking out the reactant, separating and cleaning, and drying to obtain the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material.
As a further improvement scheme, the tetraethoxysilane is subjected to polycondensation reaction in the solution to generate silicon dioxide, and the mixed solvent and the proportion thereof are adjusted to ensure that the reaction speed is consistent with the generation speed of the ferroferric oxide.
As a further improvement, the intermediate product C of the condensation polymerization of tetraethoxysilane in the solution 2 H 5 OH，C 2 H 5 OH has reducibility, so that the oxidation speed of ferrous ions is reduced, and the final product is ferroferric oxide.
As a further improvement, the ferrous ions are complexed with DMF and water, and the molecular force between the complex and tetraethoxysilane enables the two to generate adsorption. The ferrous complex is decomposed and oxidized to form ferroferric oxide. The condensation polymerization of ethyl orthosilicate produces the product silicon dioxide. The mutual inhibition of the ferroferric oxide and the silicon oxide ensures that the particle diameter of the ferroferric oxide and the silicon oxide is very small and the particles are uniformly dispersed.
As a further modification, in step S3, the mixed solution is transferred to a water bath kettle and stirred in a water bath at 90 ℃ for 2 hours; then, the mixture was taken out and stirred at room temperature for 5 minutes.
As a further improvement, in step S4, the reaction product is taken out, washed by magnetic separation with alcohol and distilled water, and dried after the alcohol is volatilized at room temperature.
The invention also discloses a magnetic core, which is formed by pressing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material or the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material prepared by the method.
As a further improvement, the magnetic core has high impedance above 200MHz and low impedance in the frequency band below 2 MHz.
Compared with the prior art, the invention has the following beneficial effects:
(1) The ethyl orthosilicate generates a polycondensation reaction in the solution to generate silicon dioxide and C 2 H 5 OH, product C therein 2 H 5 OH has reducibility, so that the oxidation speed of ferrous ions is reduced, and the final product is ferroferric oxide, so that the final product has good soft magnetic characteristics. Oxygen isolation and reducing agent addition are not needed in the reaction process.
(2) The ferrous ions are complexed with DMF and water, and the molecular force between the complex and tetraethoxysilane enables the two to generate adsorption. The ferrous complex is decomposed and oxidized to form ferroferric oxide. Condensation product silicon dioxide of ethyl orthosilicate. Due to the mutual inhibition effect, the particle diameters of the ferroferric oxide and the silicon oxide are very small, so that the silicon dioxide and the ferroferric oxide are in a nanometer level and are uniformly dispersed with each other. Wherein the silicon dioxide is amorphous, the ferroferric oxide is nanocrystalline, and the particle size is below 5nm.
(3) Because the particles are fine, the composite material can be directly pressed into a magnetic ring without adding an adhesive. The pressed magnetic ring only needs to be baked at a low temperature of 100 ℃, and the hardness of the magnetic core can be improved. The magnetic core has good high-frequency anti-interference performance, can absorb high-frequency electromagnetic waves of 200 MHz-2.5 GHz, and has impedance of more than 100 omega.
Description of the drawings:
FIG. 1 is a flow chart of the steps for preparing the composite material of the present invention.
Figure 2 XRD pattern of the composite material of the present invention.
FIG. 3 is an SEM image of a composite material of the present invention.
Fig. 4 shows a hysteresis loop of the composite material of the invention.
FIG. 5 is a magnetic loop impedance spectrum made of the composite material of the present invention.
The specific implementation mode is as follows:
in order to better explain the process and scheme of the present invention, the following invention is further described with reference to the accompanying drawings and examples. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
In order to solve the technical problems in the prior art, referring to fig. 1, a flow chart of the preparation steps of the composite material of the present invention is shown, which comprises the following steps:
step S1, measuring dimethyl formamide DMF and distilled water with a volume ratio of 8, and mixing to obtain a mixed solvent;
step S2, feCl is added 2 ·4H 2 O, tetraethoxysilane and sodium acetate, and stirring for 10 minutes at normal temperature until the O, tetraethoxysilane and sodium acetate are fully dissolved and uniformly mixed. FeCl 2 ·4H 2 The concentration of O relative to the mixed solvent is 10-15 mg/mL, the volume ratio of the ethyl orthosilicate to the mixed solvent is 0.001.
S3, transferring the mixture into a water bath kettle, stirring the mixture in water bath for 2 to 4 hours at the temperature of 90 ℃, taking the mixture out, and stirring the mixture for 5 minutes at room temperature;
and step S4, taking out the reactant, and carrying out magnetic separation and cleaning for 3 times by using distilled water and alcohol respectively. And (3) volatilizing and drying the alcohol at room temperature to obtain the amorphous nanocrystalline anti-interference material.
The following examples illustrate the preparation of the composite material of the present invention.
Example 1
Measuring 8mL of dimethylformamide DMF and 2mL of distilled water, and mixing to obtain a mixed solvent; adding 100mg FeCl 2 ·4H 2 O, 10. Mu.L of ethyl orthosilicate and 150mg of sodium acetate. Stirring for 10 minutes at normal temperature until the components are fully dissolved and uniformly mixed; transferring to a water bath kettle, stirring in water bath at 90 ℃ for 2 hours, taking out, and stirring at room temperature for 5 minutes; the reaction product was taken out and washed by magnetic separation with alcohol and distilled water. And (3) volatilizing and drying the alcohol at room temperature to obtain the amorphous nanocrystalline anti-interference material.
The XDR of the composite material prepared in example 1 was measured as shown in FIG. 2, which shows diffraction peaks of all Fe 3 O 4 The diffraction peak of (1). Fe can be observed in the figure 3 O 4 The width of the diffraction peak was very broad, and from this, fe was found 3 O 4 The grain size of (2) is very small. From the weight of the product and analysis of the product prepared with ethyl orthosilicate alone, siO was present in the material 2 Ingredients (A) are provided. Although no diffraction peak of nano-silica was found in XRD diffraction, this is because the prepared silica was amorphous. The scanning electron micrograph of the composite material is shown in FIG. 3, and it can be seen that the diameter of the composite particles is about 5nm. The prepared material was subjected to a VSM test to obtain a hysteresis loop as shown in fig. 4, and as can be seen from the hysteresis loop, the saturation magnetization of the composite material was about 35 emu/g. And has good paramagnetic properties.
The composite material obtained in example 1 was placed in a mold and pressed into an interference-free magnetic core of 12mm × 5mm × 7mm (outer diameter × inner diameter × height), and the magnetic core was placed in an oven at 100 ℃ and held for 10 hours. A wire is passed through the core and the impedance of the interference-resistant core is detected in the range of 1M-3G by an impedance analyzer. Fig. 5 shows the impedance characteristics of the composite material. The test results show that the impedance is greater than 100 omega in the interval of 200M to 2.5 GHz. And the impedance of the frequency below 2MHz is less than 1 omega, so the high-frequency anti-electromagnetic interference filter can be used for resisting high-frequency electromagnetic interference.
Example 2
Measuring 8mL of dimethylformamide DMF and 2mL of distilled water, and mixing to obtain a mixed solvent; adding 150mg FeCl 2 ·4H 2 O, 50. Mu.L of ethyl orthosilicate and 300mg of sodium acetate. Stirring for 10 minutes at normal temperature until the components are fully dissolved and uniformly mixed; transferring to a water bath kettle, stirring in water bath at 90 ℃ for 3 hours, taking out, and stirring at room temperature for 5 minutes until cooling; the reaction product was taken out and washed by magnetic separation with alcohol and distilled water. And (3) volatilizing and drying the alcohol at room temperature to obtain the amorphous nanocrystalline anti-interference material.
Example 3
Measuring 8mL of dimethylformamide DMF and 2mL of distilled water, and mixing to obtain a mixed solvent; adding 120mg FeCl 2 ·4H 2 O, 30. Mu.L of ethyl orthosilicate and 200mg of sodium acetate. Stirring for 10 min at normal temperature until the materials are fully dissolved,Mixing uniformly; transferring to a water bath kettle, stirring in water bath at 90 ℃ for 4 hours, taking out, and stirring at room temperature for 5 minutes until cooling; the reaction product was taken out and washed by magnetic separation with alcohol and distilled water. And (3) volatilizing and drying the alcohol at room temperature to obtain the amorphous nanocrystalline anti-interference material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A preparation method of an amorphous nanocrystalline high-frequency anti-interference magnetic core composite material is characterized by comprising the following steps:
step S1, measuring dimethyl formamide DMF and distilled water with a volume ratio of 8;
step S2, adding FeCl 2 ·4H 2 O, ethyl orthosilicate and sodium acetate, stirring for 10 minutes at normal temperature until the O, the ethyl orthosilicate and the sodium acetate are fully dissolved and uniformly mixed to obtain a mixed solution, wherein FeCl 2 ·4H 2 The concentration of O relative to the mixed solvent is 10 to 15mg/mL, the volume ratio of the ethyl orthosilicate to the mixed solvent is 0.001 to 1 to 0.005, and the concentration of the sodium acetate relative to the mixed solvent is 15 to 30mg/mL;
s3, stirring the mixed solution in a constant-temperature water bath for 2 to 4 hours to fully react;
s4, taking out the reactant, separating and cleaning, and drying to obtain the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material;
the prepared amorphous nanocrystalline high-frequency anti-interference magnetic core composite material is made of nanocrystalline Fe 3 O 4 And amorphous SiO 2 The nano particles are mutually and uniformly dispersed, and the particle diameters of the nano particles and the nano particles are less than 5nm.
2. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, characterized in that the composite material is prepared by a low-temperature water bath method in one step.
3. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, wherein tetraethoxysilane is subjected to polycondensation reaction in a solution to generate silicon dioxide, and the mixed solvent and the proportion thereof are adjusted to enable the reaction speed to be consistent with the generation speed of ferroferric oxide.
4. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, wherein an intermediate product of condensation polymerization reaction of ethyl orthosilicate in a solution is C 2 H 5 OH，C 2 H 5 OH has reducibility, so that the oxidation speed of ferrous ions is reduced, and the final product is ferroferric oxide.
5. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, wherein ferrous ions, DMF and water are complexed, and molecular force between the complex and tetraethoxysilane enables the complex and tetraethoxysilane to generate adsorption; decomposing and oxidizing the ferrous complex to form ferroferric oxide; condensation polymerization of ethyl orthosilicate to produce silicon dioxide; the mutual inhibition of the ferroferric oxide and the silicon oxide ensures that the particle diameter of the ferroferric oxide and the silicon oxide is very small and the particles are uniformly dispersed.
6. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, wherein in step S3, the mixed solution is transferred to a water bath kettle and stirred in a water bath at 90 ℃ for 2 hours; then, the mixture was taken out and stirred at room temperature for 5 minutes.
7. The method for preparing the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material according to claim 1, wherein in step S4, the reactant is taken out, magnetic separation and cleaning are performed by using alcohol and distilled water, and drying is performed after the alcohol is volatilized at room temperature.
8. A magnetic core, characterized in that, the amorphous nanocrystalline high-frequency anti-interference magnetic core composite material prepared by any one of the methods of claims 1 to 7 is pressed.
9. The magnetic core according to claim 8, wherein the magnetic core has an impedance of 100 Ω or more at 200mhz to 2.5ghz and an impedance of less than 1 Ω at a frequency band lower than 2 MHz.
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| US5728195A (en) * | 1995-03-10 | 1998-03-17 | The United States Of America As Represented By The Department Of Energy | Method for producing nanocrystalline multicomponent and multiphase materials |
| CN101348713A (en) * | 2007-07-20 | 2009-01-21 | 同济大学 | Magnetic composite nano microsphere capable of emitting fluorescence and preparation thereof |
| CN102489300A (en) * | 2011-11-18 | 2012-06-13 | 东华大学 | Preparation method for magnetic nanometer microballoon photocatalysis composite materials |
| CN109285998A (en) * | 2018-08-09 | 2019-01-29 | 杭州电子科技大学 | Silicon/ferrosilicon oxide/iron oxide/carbon core-shell structure material and preparation method thereof |
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| US5728195A (en) * | 1995-03-10 | 1998-03-17 | The United States Of America As Represented By The Department Of Energy | Method for producing nanocrystalline multicomponent and multiphase materials |
| CN101348713A (en) * | 2007-07-20 | 2009-01-21 | 同济大学 | Magnetic composite nano microsphere capable of emitting fluorescence and preparation thereof |
| CN102489300A (en) * | 2011-11-18 | 2012-06-13 | 东华大学 | Preparation method for magnetic nanometer microballoon photocatalysis composite materials |
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