CN114654823B - 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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- CN114654823B CN114654823B CN202210319951.XA CN202210319951A CN114654823B CN 114654823 B CN114654823 B CN 114654823B CN 202210319951 A CN202210319951 A CN 202210319951A CN 114654823 B CN114654823 B CN 114654823B
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Abstract
The invention relates to the technical field of soft magnetic alloy wave-absorbing materials, in particular to an 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 an Mn-Zn ferrite matching layer; preparing a FeSiAl wave absorbing layer; alternately superposing a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers, and then performing hot pressing to obtain an Mn-Zn ferrite-FeSiAl composite wave-absorbing material; the wave-absorbing material is designed into a multi-layer structure by utilizing the principle of gradual impedance change, the Mn-Zn ferrite layer is used as an impedance matching layer, the FeSiAl layer is used as a wave-absorbing layer, and the high impedance matching is effectively realized by respectively regulating and controlling the thicknesses of the FeSiAl layer and the Mn-Zn ferrite layer, so that 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 an Mn-Zn ferrite-FeSiAl composite wave-absorbing material and a preparation method thereof.
Background
The 5G communication network is a foundation stone for digital transformation of the whole society, and compared with 4G, the frequency band of the 5G is expanded from centimetre waves to millimeter waves, so that the data transmission speed is faster, the frequency band is higher, and the bandwidth is wider; electromagnetic wave pollution can generate interference signals in the mobile communication propagation process, so that the communication quality is affected, meanwhile, the harm of electromagnetic radiation between high-frequency components and equipment to human bodies is also becoming serious, so that how to effectively eliminate electromagnetic interference, electromagnetic radiation and other electromagnetic pollution is a key technology to be solved in the current electronic equipment for 5G communication, most of the existing wave absorbing materials are single-layer materials, and the high-performance requirements of large bandwidth and strong wave absorption are difficult to meet for the single-layer materials.
Disclosure of Invention
The invention aims to provide an Mn-Zn ferrite-FeSiAl composite wave-absorbing material and a preparation method thereof, which can be used for preparing a multi-layer FeSiAl/Mn-Zn ferrite alternating composite soft magnetic wave-absorbing material, effectively realizes high impedance matching and can 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 method for preparing a Mn-Zn ferrite-fesai composite wave-absorbing material with a large bandwidth and low reflection loss, comprising:
preparing an Mn-Zn ferrite matching layer;
preparing a FeSiAl wave absorbing layer;
and alternately superposing a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers, and then performing hot pressing to obtain the Mn-Zn ferrite-FeSiAl composite wave-absorbing material.
Wherein, the preparation of Mn-Zn ferrite matching layer comprises:
preparation of Fe 2 O 3 、Mn 3 O 4 And ZnO for standby, wherein the mol percent is as follows: fe (Fe) 2 O 3 ：Mn 3 O 4 ：ZnO＝52：25：23；
Weighing proportionally Fe 2 O 3 、Mn 3 O 4 Putting ZnO and deionized water into a ball milling tank for ball milling to obtain powder slurry;
drying the powder slurry, and preserving heat in nitrogen atmosphere after drying to obtain pure-phase Mn-Zn ferrite powder;
mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1:0.7: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.6: mixing in a proportion of 0.05, and performing secondary ball milling to obtain Mn-Zn ferrite slurry;
and carrying out tape casting molding on the Mn-Zn ferrite slurry, wherein the prepared tape casting diaphragm is the Mn-Zn ferrite matching layer.
Wherein the dispersing agent is one or a mixture of two 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:
granular Fe with grain diameter of 5-20 mu m 85 Si 9.6 Al 5.4 Placing 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 according to the proportion of 1:1.5: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.3: mixing in a proportion of 0.05, and performing secondary ball milling to obtain FeSiAl slurry;
and carrying out tape casting molding on the FeSiAl slurry, wherein the prepared tape casting diaphragm is 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 a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave absorbing layers are alternately overlapped.
According to the Mn-Zn ferrite-FeSiAl composite wave-absorbing material and the preparation method thereof, the wave-absorbing material is designed into a multi-layer structure by utilizing the principle of gradual impedance 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 alternating composite soft magnetic wave-absorbing material, takes an 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.
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In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss.
FIG. 2 is a flow chart of the preparation of Mn-Zn ferrite matching layer of the present invention.
Fig. 3 is a flow chart of the present invention for preparing a fesai wave-absorbing layer.
FIG. 4 is a schematic structural diagram of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material (total thickness 2.5 mm) of the present invention.
FIG. 5 is a RL-f curve of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material (total thickness 2.5 mm) of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not 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-fesai composite wave-absorbing material with large bandwidth and low reflection loss, which includes:
s1, preparing an Mn-Zn ferrite matching layer;
the method comprises the following specific steps:
s11 preparation of Fe 2 O 3 、Mn 3 O 4 And ZnO for standby, wherein the mol percent is as follows: fe (Fe) 2 O 3 ：Mn 3 O 4 ：ZnO＝52：25：23；
By Fe 2 O 3 (purity of 99.2% or more), mn 3 O 4 (Mn content is more than or equal to 71%), znO (purity is more than or equal to 99.7%) is used as a basic raw material, and the mol percent of the composition is as follows: fe (Fe) 2 O 3 ：Mn 3 O 4 : znO = 52:25:23; wherein Fe is 2 O 3 Purity of 99.2% or more, mn 3 O 4 The Mn content in the alloy is more than or equal to 71 percent, and ZnO (the purity is more than or equal to 99.7 percent).
S12 is to weigh Fe in proportion 2 O 3 、Mn 3 O 4 Putting ZnO and deionized water into a ball milling tank for ball milling to obtain powder slurry;
weighing the ingredients according to the designed components, and weighing the weighed Fe 2 O 3 、Mn 3 O 4 Putting ZnO and ZnO into a ball milling tank, addingAnd (3) adding deionized water for ball milling, wherein the ball milling time is 4 hours, and the rotating speed is set to be 250r/min.
S13, drying the powder slurry, and preserving heat in a nitrogen atmosphere after drying to obtain pure-phase Mn-Zn ferrite powder;
and (3) drying the powder slurry in a drying oven at 80 ℃ for a plurality of hours, and then carrying out heat preservation on the dried powder at 1000 ℃ for 3 hours under nitrogen atmosphere to prepare the pure-phase Mn-Zn ferrite powder.
S14, mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1:0.7: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.6: mixing in a proportion of 0.05, and performing secondary ball milling to obtain 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, performing ball milling once, wherein the ball milling rotating speed is 280r/min, the ball milling time is 1h, and preparing magnetic powder, and on the basis, performing ball milling according to the following steps: and (2) a binder: plasticizer = 1:0.6: and 0.05, respectively adding a binder and a plasticizer into the magnetic powder, performing secondary ball milling at the ball milling rotation speed of 280r/min for 1h, sieving through a 80-mesh screen and a 200-mesh screen respectively after the mixed slurry is obtained, and performing vacuum defoaming on the sieved slurry, wherein the viscosity of the slurry is 280-450 mPa.s, thus obtaining the Mn-Zn ferrite slurry. Wherein the dispersing agent is one or a mixture of two of tributyl phosphate and triethanolamine, the binder is polyvinyl butyral, and the plasticizer is dibutyl phthalate.
S15, carrying out tape casting molding on the Mn-Zn ferrite slurry, wherein the prepared tape casting diaphragm is the Mn-Zn ferrite matching layer;
pouring Mn-Zn iron to prepare oxygen slurry on PET film with baffles at two sides of a casting machine, adjusting the thickness of the doctor-blade slurry by utilizing the clearance between a doctor blade and the PET film, setting the height of the doctor blade to be 500 mu m, casting at the speed of about 60mm/min, continuously doctor-blade-coating a uniform film strip by the traction of the PET film, and drying at normal temperature. Forming a casting film with the thickness of 50 mu m, rolling for standby, and preparing the Mn-Zn ferrite matching layer.
S2, preparing a FeSiAl wave-absorbing layer;
the method comprises the following specific steps:
s21 particulate Fe having a particle diameter of 5 to 20 [ mu ] m 85 Si 9.6 Al 5.4 Placing 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 particle diameter of 5-20 mu m 85 Si 9.6 Al 5.4 And (3) placing the magnetic powder into a ball milling tank, adding deionized water for ball milling for 4 hours, setting the rotating speed to be 250r/min, placing the ball-milled slurry into a blast drying oven for drying, and obtaining the sheet FeSiAl magnetic powder.
S22, mixing the sheet FeSiAl magnetic powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1:1.5: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.3: mixing in a proportion of 0.05, and performing secondary ball milling to obtain FeSiAl slurry;
triethanolamine is used as a dispersing agent, and the sheet FeSiAl magnetic powder, absolute ethyl alcohol and the dispersing agent are mixed according to the following weight ratio of 1:1.5: weighing in a proportion of 0.025, performing ball milling once, wherein the ball milling rotating speed is 250r/min, the ball milling time is 1h, and preparing magnetic powder, on the basis, taking polyvinyl butyral (PVB) as a binder, taking dibutyl phthalate (DBP) as a plasticizer, and mixing the following magnetic powder: and (2) a binder: plasticizer = 1:0.3: and respectively adding a binder and a plasticizer into the magnetic powder according to the proportion of 0.05, performing secondary ball milling at the ball milling rotating speed of 250r/min for 1h to obtain mixed slurry, sieving the mixed slurry through a 80-mesh screen and a 200-mesh screen respectively, and performing vacuum defoaming on the sieved slurry to obtain FeSiAl slurry.
S23, carrying out tape casting molding on the FeSiAl slurry, wherein the prepared tape casting membrane is a FeSiAl wave absorbing layer;
pouring the prepared FeSiAl slurry on PET films with baffles at two sides of a casting machine, adjusting the thickness of the doctor-blading slurry by utilizing the clearance between a doctor blade and the PET films, setting the height of the doctor blade to be 500 mu m, and continuously doctor-blading a uniform film strip by the traction of the PET films at the casting speed of about 60mm/min, drying at normal temperature to form a casting film with the thickness of 100 mu m, and rolling for standby to prepare the FeSiAl wave-absorbing layer.
S3, alternately superposing a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers, and then performing hot pressing to obtain an Mn-Zn ferrite-FeSiAl composite wave-absorbing material;
cutting the prepared Mn-Zn ferrite matching layer and FeSiAl wave-absorbing layer green tape into 20X 20mm, alternately superposing multiple layers, and hot-pressing at 25MPa and 100 ℃ for 30min to obtain Mn-Zn ferrite-FeSiAl composite wave-absorbing material samples.
According to the preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss, the wave-absorbing material is designed into a multi-layer structure by utilizing the principle of gradual impedance 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 alternating composite soft magnetic wave-absorbing material, takes an Mn-Zn ferrite layer as an impedance matching layer and a FeSiAl layer as a wave-absorbing layer, effectively realizes high impedance matching by respectively regulating and controlling the thicknesses of the FeSiAl layer and the Mn-Zn ferrite layer, and obtains the Mn-Zn ferrite/FeSiAl composite soft magnetic wave-absorbing material with large bandwidth and low reflection loss;
referring to fig. 4 and 5, the electromagnetic parameters of the wave-absorbing material are analyzed and measured by a vector network analyzer, and the multilayer reflection loss is calculated by the 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 (15.9 GHz) 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 (11.7 GHz-18 GHz).
Therefore, compared with the existing material, the invention has the following beneficial effects: the Mn-Zn ferrite/FeSiAl composite material prepared by the invention has obviously improved wave absorbing performance, the RL is less than or equal to-10 dB, and the effective absorption bandwidth is more than or equal to 6GHz; meanwhile, the impedance matching of Mn-Zn ferrite and 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 invention adopts the casting method technology process to prepare the Mn-Zn ferrite/FeSiAl composite soft magnetic wave-absorbing material, has simple flow and can be produced in large scale.
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 a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave absorbing layers are alternately overlapped.
In the embodiment, the multi-layer FeSiAl/Mn-Zn ferrite alternating composite soft magnetic wave-absorbing material is constructed by designing the wave-absorbing material into a multi-layer structure, 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, and the high impedance matching is effectively realized by respectively regulating and controlling the thicknesses of the Mn-Zn ferrite matching layer and the FeSiAl wave-absorbing layer, so that the Mn-Zn ferrite/FeSiAl composite soft magnetic wave-absorbing material with large bandwidth and low reflection loss is obtained.
The above disclosure is only a preferred embodiment of the present invention, and it should be understood that the scope of the invention is not limited thereto, and those skilled in the art will appreciate that all or part of the procedures described above can be performed according to the equivalent changes of the claims, and still fall within the scope of the present invention.
Claims (5)
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 an Mn-Zn ferrite matching layer;
preparing a FeSiAl wave absorbing layer;
alternately superposing a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave-absorbing layers, and then performing hot pressing to obtain an Mn-Zn ferrite-FeSiAl composite wave-absorbing material;
the preparation of the Mn-Zn ferrite matching layer comprises the following steps:
preparation of Fe 2 O 3 、Mn 3 O 4 For standby with ZnO, the mole percentage is Fe 2 O 3 ：Mn 3 O 4 ：ZnO=52：25：23；
Weighing proportionally Fe 2 O 3 、Mn 3 O 4 Putting ZnO and deionized water into a ball milling tank for ball milling to obtain powder slurry;
drying the powder slurry, and preserving heat in nitrogen atmosphere after drying to obtain pure-phase Mn-Zn ferrite powder;
mixing the Mn-Zn ferrite powder, absolute ethyl alcohol and a dispersing agent according to the proportion of 1:0.7: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.6: mixing in a proportion of 0.05, and performing secondary ball milling to obtain Mn-Zn ferrite slurry;
carrying out tape casting molding on the Mn-Zn ferrite slurry, wherein the prepared tape casting diaphragm is the Mn-Zn ferrite matching layer;
the preparation of the FeSiAl wave-absorbing layer comprises the following steps:
granular Fe with particle diameter of 5-20 mu m 85 Si 9.6 Al 5.4 Placing 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 according to the proportion of 1:1.5: mixing the materials according to the proportion of 0.025, performing ball milling for the first time to obtain magnetic powder, and mixing the magnetic powder, the binder and the plasticizer according to the proportion of 1:0.3: mixing in a proportion of 0.05, and performing secondary ball milling to obtain FeSiAl slurry;
and carrying out tape casting molding on the FeSiAl slurry, wherein the prepared tape casting diaphragm is the FeSiAl wave absorbing layer.
2. The method for preparing the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss as claimed in claim 1, wherein,
the dispersing agent is one or a mixture of two of tributyl phosphate and triethanolamine.
3. The method for preparing the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss as claimed in claim 1, wherein,
the binder is polyvinyl butyral.
4. The method for preparing the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss as claimed in claim 1, wherein,
the plasticizer is dibutyl phthalate.
5. A Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss is prepared by the preparation method of the Mn-Zn ferrite-FeSiAl composite wave-absorbing material with large bandwidth and low reflection loss according to any one of claims 1-4,
comprises a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave absorbing layers; and a plurality of Mn-Zn ferrite matching layers and a plurality of FeSiAl wave absorbing layers are alternately overlapped.
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| CN109664567A (en) * | 2018-12-12 | 2019-04-23 | 横店集团东磁股份有限公司 | A kind of thermally conductive Wave suction composite material of sheet type and preparation method thereof |
| CN111171508A (en) * | 2020-03-06 | 2020-05-19 | 苏州世华新材料科技股份有限公司 | Temperature-resistant wave-absorbing material and preparation method thereof |
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