CN114654823A - Mn-Zn ferrite-FeSiAl composite wave-absorbing material and preparation method thereof - Google Patents
Mn-Zn ferrite-FeSiAl composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of soft magnetic alloy wave-absorbing materials, in particular to a Mn-Zn ferrite-FeSiAl composite wave-absorbing material and a preparation method thereof, wherein the preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss comprises the following steps: preparing a Mn-Zn ferrite matching layer; preparing a FeSiAl wave absorbing layer; alternately superposing the multiple Mn-Zn ferrite matching layers and the multiple FeSiAl wave-absorbing layers and then carrying out hot pressing to prepare the Mn-Zn ferrite-FeSiAl composite wave-absorbing material; by utilizing the principle of impedance gradual change, the wave-absorbing material is designed into a multilayer structure, the Mn-Zn ferrite layer is used as an impedance matching layer, the FeSiAl layer is used as a wave-absorbing layer, and the thicknesses of the FeSiAl layer and the Mn-Zn ferrite layer are respectively regulated and controlled, so that high impedance matching is effectively realized, and the Mn-Zn ferrite/FeSiAl composite soft magnetic wave-absorbing material with large bandwidth and low reflection loss is obtained.
Description
Technical Field
The invention relates to the technical field of soft magnetic alloy wave-absorbing materials, in particular to a Mn-Zn ferrite-FeSiAl composite wave-absorbing material and a preparation method thereof.
Background
The 5G communication network is a cornerstone of the whole social digital transformation, compared with the 4G communication network, the frequency band of the 5G communication network is expanded from centimeter waves to millimeter waves, and the data transmission speed is higher, the frequency band is higher, and the bandwidth is wider; electromagnetic wave pollution can produce interference signal in mobile communication propagation process, thereby influence communication quality, meanwhile, electromagnetic radiation between high frequency components and parts and the equipment is also growing seriously to the harm of human body, consequently, how effectively to eliminate electromagnetic pollution such as electromagnetic interference and electromagnetic radiation has become the key technology that present 5G communication electronic equipment waited for a short time to solve, current absorbing material is the individual layer material mostly, to the individual layer material, be difficult to satisfy the big bandwidth, the high performance demand of strong ripples.
Disclosure of Invention
The invention aims to provide a Mn-Zn ferrite-FeSiAl composite wave-absorbing material and a preparation method thereof, which can be used for preparing a multilayer FeSiAl/Mn-Zn ferrite alternating composite soft magnetic wave-absorbing material, effectively realize high impedance matching and meet the high performance requirements of large bandwidth and strong wave absorption.
In order to achieve the above object, in a first aspect, the present invention provides a preparation method of a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with a large bandwidth and a low reflection loss, comprising:
preparing a Mn-Zn ferrite matching layer;
preparing a FeSiAl wave absorbing layer;
and alternately superposing the multiple Mn-Zn ferrite matching layers and the multiple FeSiAl wave-absorbing layers, and then carrying out hot pressing to obtain the Mn-Zn ferrite-FeSiAl composite wave-absorbing material.
Wherein the preparing the Mn-Zn ferrite matching layer comprises:
preparation of Fe2O3、Mn3O4And ZnO for standby, the mol percentage is as follows: fe2O3：Mn3O4：ZnO＝52：25：23；
Proportionally weighing Fe2O3、Mn3O4Putting ZnO and ZnO into a ball milling tank, adding deionized water, and ball milling to obtain powder slurry;
drying the powder slurry, and then preserving heat in a nitrogen atmosphere to prepare pure-phase Mn-Zn ferrite powder;
mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent in a proportion of 1:0.7:0.025, and performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to a ratio of 1: 0.6: mixing the materials in a proportion of 0.05, and performing secondary ball milling to prepare Mn-Zn ferrite slurry;
and carrying out tape casting on the Mn-Zn ferrite slurry to obtain a tape casting film, namely the Mn-Zn ferrite matching layer.
Wherein the dispersant is one or a mixture of tributyl phosphate and triethanolamine.
Wherein the binder is polyvinyl butyral.
Wherein the plasticizer is dibutyl phthalate.
Wherein, the preparation of the FeSiAl wave-absorbing layer comprises the following steps:
the granular Fe with the grain diameter of 5-20 mu m85Si9.6Al5.4Putting the magnetic powder into a ball milling tank, adding deionized water for ball milling, and drying the slurry after ball milling to obtain sheet FeSiAl magnetic powder;
mixing the sheet FeSiAl magnetic powder, absolute ethyl alcohol and a dispersing agent in a proportion of 1: 1.5: mixing the raw materials according to the proportion of 0.025, performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to the proportion of 1: 0.3: mixing the raw materials according to the proportion of 0.05, and performing secondary ball milling to prepare FeSiAl slurry;
and carrying out tape casting on the FeSiAl slurry to obtain a tape casting membrane, namely the FeSiAl wave absorbing layer.
In a second aspect, the invention also provides a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss, which comprises a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers; and the Mn-Zn ferrite matching layers and the FeSiAl wave-absorbing layers are alternately superposed.
According to the Mn-Zn ferrite-FeSiAl composite wave-absorbing material and the preparation method thereof, the wave-absorbing material is designed into a multilayer structure by utilizing the principle of impedance gradual change, the Mn-Zn ferrite is a matching layer, and the FeSiAl is a high-loss layer. The invention constructs a multilayer FeSiAl/Mn-Zn ferrite alternate composite soft magnetic wave absorbing material, takes a Mn-Zn ferrite layer as an impedance matching layer and a FeSiAl layer as a wave absorbing layer, and effectively realizes high impedance matching by respectively regulating and controlling the thicknesses of the FeSiAl layer and the Mn-Zn ferrite layer, thereby obtaining the Mn-Zn ferrite/FeSiAl composite soft magnetic wave absorbing material with large bandwidth and low reflection loss.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a preparation method of a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss.
FIG. 2 is a flow chart of the present invention for preparing a Mn-Zn ferrite matching layer.
FIG. 3 is a flow chart of the preparation of FeSiAl wave-absorbing layer according to the present invention.
FIG. 4 is a schematic structural view of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material (total thickness 2.5mm) of the invention.
FIG. 5 is an RL-f curve of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material (total thickness is 2.5 mm).
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
Referring to fig. 1 to 5, in a first aspect, the present invention provides a method for preparing a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with a large bandwidth and a low reflection loss, including:
s1, preparing a Mn-Zn ferrite matching layer;
the method comprises the following specific steps:
s11 preparation of Fe2O3、Mn3O4And ZnO for standby, the mol percentage is: fe2O3：Mn3O4：ZnO＝52：25：23；
Using Fe2O3(purity not less than 99.2%), Mn3O4(Mn content is more than or equal to 71 percent) and ZnO (purity is more than or equal to 99.7 percent) are used as basic raw materials, and the mol percentage of the components is as follows: fe2O3：Mn3O4: ZnO-52: 25: 23; wherein, Fe2O3Purity of 99.2% or more and Mn3O4The Mn content is greater than or equal to 71 percent, and the ZnO (the purity is greater than or equal to 99.7 percent).
S12 proportionally weighing Fe2O3、Mn3O4Putting ZnO and ZnO into a ball milling tank, adding deionized water, and ball milling to obtain powder slurry;
proportioning and weighing the materials according to the designed components, and weighing the weighed Fe2O3、Mn3O4And ZnO is put into a ball milling tank, deionized water is added for ball milling, the ball milling time is 4 hours, and the rotating speed is set to be 250 r/min.
S13, drying the powder slurry, and keeping the temperature in a nitrogen atmosphere to obtain pure-phase Mn-Zn ferrite powder;
and drying the powder slurry in a drying oven at 80 ℃ for a plurality of hours, and then preserving the temperature of the dried powder for 3 hours at 1000 ℃ under nitrogen atmosphere to prepare pure-phase Mn-Zn ferrite powder.
S14, mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent in a proportion of 1:0.7:0.025, and performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to a ratio of 1: 0.6: mixing the materials according to the proportion of 0.05, and performing secondary ball milling to prepare Mn-Zn ferrite slurry;
weighing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1:0.7:0.025, carrying out primary ball milling, wherein the ball milling rotation speed is 280r/min, the ball milling time is 1h, and preparing magnetic powder, wherein on the basis, the proportion of the magnetic powder is as follows: adhesive: plasticizer 1: 0.6: 0.05 respectively adding a binder and a plasticizer into the magnetic powder, carrying out secondary ball milling, wherein the ball milling rotation speed is 280r/min, the ball milling time is 1h, obtaining mixed slurry, sieving the mixed slurry through 80-mesh and 200-mesh screens, and removing bubbles from the sieved slurry in vacuum, wherein the viscosity of the slurry is 280-450 mPa & s, thus obtaining the Mn-Zn ferrite slurry. The dispersing agent is one or a mixture of tributyl phosphate and triethanolamine, the binder is polyvinyl butyral, and the plasticizer is dibutyl phthalate.
S15, carrying out tape casting on the Mn-Zn ferrite slurry to obtain a tape casting film, namely an Mn-Zn ferrite matching layer;
pouring ferrite slurry prepared from Mn-Zn iron on a PET film with baffles at two sides of a casting machine, adjusting the thickness of blade coating slurry by utilizing the gap between a scraper and the PET film, setting the height of the scraper to be 500 mu m, setting the casting speed to be about 60mm/min, continuously blade-coating a uniform film strip by drawing the PET film, and drying at normal temperature. And forming a casting film with the thickness of 50 mu m, and rolling up for later use to prepare the Mn-Zn ferrite matching layer.
S2, preparing a FeSiAl wave absorbing layer;
the method comprises the following specific steps:
s21 granular Fe with the grain diameter of 5-20 mu m85Si9.6Al5.4Putting the magnetic powder into a ball milling tank, adding deionized water for ball milling, and drying the slurry after ball milling to obtain sheet FeSiAl magnetic powder;
granular Fe with the grain diameter of 5-20 mu m85Si9.6Al5.4And putting the magnetic powder into a ball milling tank, adding deionized water for ball milling for 4 hours at the rotating speed of 250r/min, and putting the slurry after ball milling into a forced air drying oven for drying to obtain the sheet FeSiAl magnetic powder.
S22, mixing the flake FeSiAl magnetic powder, absolute ethyl alcohol and a dispersing agent according to the weight ratio of 1: 1.5: mixing the raw materials according to the proportion of 0.025, performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to the proportion of 1: 0.3: mixing the raw materials according to the proportion of 0.05, and performing secondary ball milling to prepare FeSiAl slurry;
taking triethanolamine as a dispersant, and mixing the flake FeSiAl magnetic powder, absolute ethyl alcohol and the dispersant according to the weight ratio of 1: 1.5: weighing 0.025 proportion, performing ball milling for one time, wherein the ball milling rotating speed is 250r/min, the ball milling time is 1h, preparing magnetic powder, and on the basis, taking polyvinyl butyral (PVB) as a binder, dibutyl phthalate (DBP) as a plasticizer, and mixing the magnetic powder: adhesive: plasticizer ═ 1: 0.3: and respectively adding a binder and a plasticizer into the magnetic powder according to the proportion of 0.05, carrying out secondary ball milling, wherein the ball milling rotation speed is 250r/min, the ball milling time is 1h, obtaining mixed slurry, sieving the mixed slurry through screens of 80 meshes and 200 meshes in sequence, and removing bubbles of the sieved slurry in vacuum to obtain the FeSiAl slurry.
S23, carrying out tape casting on the FeSiAl slurry to obtain a tape casting membrane, namely the FeSiAl wave-absorbing layer;
pouring the prepared FeSiAl slurry onto a PET film with baffles on two sides of a casting machine, adjusting the thickness of the coating slurry by utilizing the gap between a scraper and the PET film, setting the height of the scraper to be 500 mu m, setting the casting speed to be about 60mm/min, continuously coating a uniform film belt by drawing the PET film, drying at normal temperature to form a casting film with the thickness of 100 mu m, and rolling up for later use to prepare the FeSiAl wave-absorbing layer.
S3, alternately superposing the multiple Mn-Zn ferrite matching layers and the multiple FeSiAl wave-absorbing layers, and then carrying out hot pressing to obtain the Mn-Zn ferrite-FeSiAl composite wave-absorbing material;
cutting the prepared Mn-Zn ferrite matching layer and the FeSiAl wave absorbing layer into 20 multiplied by 20mm in raw belt size, alternately stacking the plurality of layers, and carrying out hot pressing at 100 ℃ under 25MPa for 30min to obtain a Mn-Zn ferrite-FeSiAl composite wave absorbing material sample.
The invention relates to a preparation method of a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss. The multilayer FeSiAl/Mn-Zn ferrite alternate composite soft magnetic wave absorbing material is constructed, the Mn-Zn ferrite layer is used as an impedance matching layer, the FeSiAl layer is used as a wave absorbing layer, the thicknesses of the FeSiAl layer and the Mn-Zn ferrite layer are respectively regulated and controlled, high impedance matching is effectively realized, and the Mn-Zn ferrite/FeSiAl composite soft magnetic wave absorbing material with large bandwidth and low reflection loss is obtained;
referring to fig. 4 and 5, a vector network analyzer is adopted to analyze and measure the electromagnetic parameters of the wave-absorbing material, and the multilayer reflection loss of the wave-absorbing material is obtained through the calculation of a coaxial line theory, when the thickness of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material is 2.5mm, the lowest reflection loss value of-19.35 dB (15.9GHz) can be obtained within the frequency range of 2-18 GHz, and the effective absorption bandwidth with the reflection loss lower than-10 dB is 6.3GHz (11.7GHz-18 GHz).
Therefore, compared with the existing material, the invention has the advantages that: the wave absorbing performance of the Mn-Zn ferrite/FeSiAl composite material prepared by the invention is obviously improved, the RL is less than or equal to-10 dB, and the effective absorption bandwidth is more than or equal to 6 GHz; meanwhile, the impedance matching of the Mn-Zn ferrite and the free space is realized, and the Mn-Zn ferrite/FeSiAl composite soft magnetic wave absorbing material with large bandwidth and low reflection loss is obtained. The manganese-zinc ferrite/FeSiAl composite soft magnetic wave-absorbing material is prepared by adopting a tape casting technology, the process is simple, and large-scale production can be realized.
In a second aspect, the invention also provides a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss, which comprises a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers; and the Mn-Zn ferrite matching layers and the FeSiAl wave-absorbing layers are alternately superposed.
In the embodiment, the wave-absorbing material is designed into a multilayer structure, so that a multilayer FeSiAl/Mn-Zn ferrite alternate composite soft magnetic wave-absorbing material is constructed, the Mn-Zn ferrite matching layer is used as an impedance matching layer, the FeSiAl wave-absorbing layer is used as a wave-absorbing layer, the thicknesses of the Mn-Zn ferrite matching layer and the FeSiAl wave-absorbing layer are respectively regulated and controlled, high impedance matching is effectively realized, and the Mn-Zn ferrite/FeSiAl composite soft magnetic wave-absorbing material with large bandwidth and low reflection loss is obtained.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss is characterized by comprising the following steps:
preparing a Mn-Zn ferrite matching layer;
preparing a FeSiAl wave absorbing layer;
and alternately superposing the multiple Mn-Zn ferrite matching layers and the multiple FeSiAl wave-absorbing layers, and then carrying out hot pressing to obtain the Mn-Zn ferrite-FeSiAl composite wave-absorbing material.
2. The preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to claim 1,
the preparation of the Mn-Zn ferrite matching layer comprises the following steps:
preparation of Fe2O3、Mn3O4And ZnO for standby, the mol percent is Fe2O3：Mn3O4：ZnO＝52：25：23；
Proportionally weighing Fe2O3、Mn3O4Putting ZnO and ZnO into a ball milling tank, adding deionized water, and ball milling to obtain powder slurry;
drying the powder slurry, and then preserving heat in a nitrogen atmosphere to prepare pure-phase Mn-Zn ferrite powder;
mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent in a proportion of 1:0.7: mixing the raw materials according to the proportion of 0.025, performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to the proportion of 1: 0.6: mixing the materials according to the proportion of 0.05, and performing secondary ball milling to prepare Mn-Zn ferrite slurry;
and carrying out tape casting on the Mn-Zn ferrite slurry to obtain a tape casting film, namely the Mn-Zn ferrite matching layer.
3. The preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to claim 2,
the dispersant is one or a mixture of tributyl phosphate and triethanolamine.
4. The preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to claim 2,
the binder is polyvinyl butyral.
5. The preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to claim 2,
the plasticizer is dibutyl phthalate.
6. The preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to claim 1,
the preparation of the FeSiAl wave-absorbing layer comprises the following steps:
mixing granular Fe with the grain diameter of 5-20 mu m85Si9.6Al5.4Putting the magnetic powder into a ball milling tank, adding deionized water for ball milling, and drying the slurry subjected to ball milling to obtain sheet FeSiAl magnetic powder;
mixing the sheet FeSiAl magnetic powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1: 1.5: mixing the raw materials according to the proportion of 0.025, performing primary ball milling to prepare magnetic powder, and mixing the magnetic powder, a binder and a plasticizer according to the proportion of 1: 0.3: mixing the raw materials according to the proportion of 0.05, and performing secondary ball milling to prepare FeSiAl slurry;
and carrying out tape casting on the FeSiAl slurry to obtain a tape casting membrane, namely the FeSiAl wave absorbing layer.
7. A Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss is prepared by applying the preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss as claimed in any one of claims 1 to 6,
comprises a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers; and the Mn-Zn ferrite matching layers and the FeSiAl wave-absorbing layers are alternately superposed.
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