CN115842248A - High-temperature-resistant soft magnetic composite wave-absorbing material and preparation method thereof - Google Patents
High-temperature-resistant soft magnetic composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of wave-absorbing material preparation, in particular to the field of IPC H05K 9/00; the interaction of the graphene and the carbonyl iron powder can widen the wave absorption frequency band, and the impedance matching degree of electromagnetic waves after the FeSi65 soft magnetic alloy powder acrylic resin is mixed is the best; the high-temperature hot pressing in the invention can ensure that materials of all layers are uniformly contacted, and the conductivity of a conducting layer in the composite material is reduced; the invention overcomes the alloy powder sedimentation effect in the mixing process of the resin and the alloy powder; the surface roughness of the semi-finished product obtained by high-temperature hot pressing is 1mm, the semi-finished product is more smooth and durable, and the problem of material loss in use is solved.
Description
Technical Field
The invention relates to the technical field of wave-absorbing material preparation, in particular to the field of IPC H05K9/00, and more particularly relates to a magnetic multilayer composite wave-absorbing material and a preparation method thereof.
Background
With the development of modern science and technology, the wave-absorbing material is applied to the surface of military equipment, can absorb detection electric waves, realizes anti-radar reconnaissance, is applied to the field of aerospace equipment, can effectively avoid electric wave interference among radars, and realizes accurate radar monitoring; the wave-absorbing material is applied to high-power electromagnetic equipment, so that the harm of electromagnetic waves to human bodies can be effectively protected; however, the existing wave-absorbing material has the defects of narrow absorption frequency band, poor physical and chemical properties, heavy weight and the like.
Chinese patent CN201711298646 discloses a broadband composite wave-absorbing material containing thermal expansion graphene, wherein the composite wave-absorbing material takes epoxy resin as a substrate, and a filling material takes thermal expansion graphene, carbon fiber, carbonyl iron powder and nickel copper ferrite composite nano-materials, and the composite wave-absorbing material with uniformly distributed fillers is prepared by vacuum defoaming. However, the absorption waveband of the composite wave-absorbing material is still narrow at 2-20 GHz.
Chinese patent CN201911153446 discloses a preparation method of magnetic wave-absorbing resin; the magnetic wave-absorbing resin is prepared by mixing and ball-milling a magnetic absorbent and graphene according to a certain mass ratio, mixing the obtained composite modified material with resin and a resin curing agent, and obtaining the flat-plate-shaped magnetic wave-absorbing resin by using a mould pressing method. However, the magnetic permeability performance of the magnetic material is not tested, and the magnetic performance cannot be judged.
Chinese patent CN201611049481 discloses a silicone oil magnetic fluid wave-absorbing material based on carboxyl siloxane and a preparation method thereof; the magnetic fluid composite coating comprises a magnetic fluid composite coating and a semiconductor coating, wherein the magnetic fluid composite coating is prepared from raw materials of Fe3O4 nano particles, graphene, carboxyl siloxane, dimethyl silicone oil, epoxy resin, ethylenediamine, carbonyl nickel powder, carbonyl iron powder or iron-based alloy magnetic powder high-magnetic-conductivity alloy powder; the semiconductor coating material comprises epoxy resin, ethylenediamine and semiconductor SiC powder; however, this material has poor heat resistance at high temperatures, and is not suitable for use in high-temperature environments.
Disclosure of Invention
The invention provides a high-temperature-resistant soft magnetic composite wave-absorbing material, which comprises a microwave-absorbing layer, a high-frequency wave-absorbing layer, a low-frequency wave-absorbing layer and a metal layer composite structure from top to bottom; the wave absorbing frequency band of the microwave absorbing layer is 10GHz-40GHz, the wave absorbing frequency band of the high-frequency wave absorbing layer is 1GHz-10GHz, and the wave absorbing frequency band of the low-frequency wave absorbing layer is 100MHz-1GHz.
Preferably, the microwave absorbing layer is prepared from the following raw materials in percentage by mass: 35-50% carbonyl iron powder, 1-2% graphene powder, and the balance first resin particles.
The preferable weight ratio of the carbonyl iron powder to the graphene powder is 45.
Preferably, the first resin particles are TPU resin; further, the TPU resin is RH4037 which is purchased from Hua-industry plastic raw material Co., ltd, innovation of Dongguan city,
preferably, the graphene powder is honeycomb layered graphene powder, further, the average particle size of the graphene powder is 20-200nm, further preferably the average particle size of the graphene powder is 100nm, and the graphene powder is purchased from pioneer nano material science and technology limited company;
preferably, the carbonyl iron powder has an average particle size of 0.1-10 μm, and a further preferred carbonyl iron powder has an average particle size of 10 μm, which is purchased from new Wuhan Diamond materials, inc.;
preferably, the high-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 60-80% of the FeSi65 soft magnetic alloy powder, and the balance of the second resin particles.
In a preferred embodiment the mass ratio of the FeSi65 magnetically soft alloy powder to the balance of the second resin particles is 7:3.
preferably, the average particle size of the FeSi65 soft magnetic alloy powder is 90-100 nm, and the average particle size of the FeSi65 soft magnetic alloy powder is 95nm, and is purchased from Beijing Yijin New Material Co.
The present inventors considered that the best impedance matching is achieved because the particle size of the soft magnetic alloy powder is uniformly mixed with a specific epoxy resin, while the impedance matching of the electromagnetic wave is best when the particle size of the FeSi65 soft magnetic alloy powder is 95nm, while the particle size of the FeSi65 soft magnetic alloy powder is 100 to 120nm in the prior art.
Preferably, the second resin is acrylic resin, the acrylic resin is thermosetting acrylic resin Setalux 1762, and the thermosetting acrylic resin Setalux 1762 is purchased from Kyowa Kay chemical Co., ltd.
Preferably, the low-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 80-90% of FeSiAl soft magnetic alloy powder and third resin particles.
Further, the mass ratio of the FeSiAl soft magnetic alloy powder to the third resin particles is 85.
The preferred average grain size of the FeSiAl soft magnetic alloy powder is 90-100 nm, and the average grain size of the FeSiAl soft magnetic alloy powder is 95nm and is purchased from Shanghai Kai-Yin chemical Co., ltd.
Preferably, the third resin particles are epoxy resin, and further, the epoxy resin is epoxy EP-12 resin particles; the epoxy EP-12 resin pellets are available from Rikawa Water, environmental industries, inc.
Preferably, the metal layer composite structure material comprises one or more of copper foil, aluminum foil, conductive cloth and conductive film, the metal layer composite structure material is preferably copper foil, and further the copper foil is 1.0mm in thickness and is purchased from Shanghai Hongyu metal material Co.
The invention also discloses a preparation method of the high-temperature resistant soft magnetic multilayer composite wave-absorbing material, which is characterized by comprising the following steps: comprises the following steps
S1, each layer is respectively subjected to glue mixing, coating and slicing to form a semi-finished product of a microwave absorbing layer, a high-frequency absorbing layer and a low-frequency absorbing layer.
S2: and then the metal layer composite structure and the metal layer composite structure are sequentially overlapped together for high-temperature hot-pressing bonding.
Further, the coating process is blade coating.
Preferably, the glue mixing process uses a ZH-1600 glue mixer produced by the automated technology Limited, dongguan, a 1200-type blade coater produced by the Pentay packaging machinery Limited, longhong, and the high-temperature hot-pressing equipment uses an HBSCR- (600-2000) t hot press produced by the Qingdao Huabo mechanical technology Limited to perform hot pressing.
The particle size of the second layer of FeSi65 soft magnetic alloy powder in the multi-layer composite wave-absorbing material is 95nm, and the particle size of the second layer of FeSiAl soft magnetic alloy powder can be 95nm in the high-temperature hot-pressing process, so that the materials of all layers can be uniformly contacted, the heat conduction capability between the layers can dissipate heat in time, and the electric conductivity of a conducting layer in the composite material can be increased due to the reduction of the temperature. The weight ratio of the epoxy resin EP-12 particles to the FeSiAl soft magnetic alloy powder is 15 to 85, so that the alloy powder can be uniformly dispersed in the resin, and the sedimentation effect of the alloy powder in the mixing process of the epoxy resin EP-12 particles and the FeSiAl soft magnetic alloy powder is overcome. According to the invention, the surface roughness of the first layer of layered honeycomb graphene material is 1mm after the first layer of layered honeycomb graphene material and the second layer of soft magnetic alloy with the grain size of 95nm FeSi65 are combined, so that the layered honeycomb graphene material is smoother and more durable, and the problem of material loss in use is solved.
Has the advantages that:
1. the interaction between the graphene and the carbonyl iron powder can widen the wave absorption frequency band.
2. The FeSi65 soft magnetic alloy powder acrylic resin has the best impedance matching degree of electromagnetic waves after being mixed.
3. The high-temperature hot pressing in the invention can ensure that materials of all layers are uniformly contacted, and the conductivity of a conducting layer in the composite material is reduced.
4. The invention overcomes the alloy powder sedimentation effect in the mixing process of the resin and the alloy powder.
5. The surface roughness of the semi-finished product obtained by high-temperature hot pressing is 1mm, the semi-finished product is more smooth and durable, and the problem of material loss in use is solved.
Examples
Example 1
The embodiment 1 of the invention discloses a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material which comprises the following components in parts by weight: the microwave absorbing material comprises a microwave absorbing layer, a high-frequency absorbing layer, a low-frequency absorbing layer and a metal layer composite structure from top to bottom; the wave absorbing frequency band of the microwave absorbing layer is 10GHz-40GHz, the wave absorbing frequency band of the high-frequency wave absorbing layer is 1GHz-10GHz, and the wave absorbing frequency band of the low-frequency wave absorbing layer is 100MHz-1GHz.
The microwave absorbing layer comprises the following raw materials in percentage by mass: 35% carbonyl iron powder (average particle size of 10 μm from new wuhan diamond material co., ltd.), 1% graphene powder (average particle size of 100nm pioneer nanomaterial science ltd.), and the balance TPU resin (RH 4037 particles from new wuhan diamond material co., ltd.).
The high-frequency wave-absorbing layer comprises the following raw materials in percentage by mass: 60% by weight of FeSi65 soft magnetic alloy powder (average particle diameter 95nm, available from Beijing Yijin New materials Co., ltd.), and the balance of thermosetting acrylic resin particles (Setalux 1762 available from Shanghai Kai Yin chemical Co., ltd.).
The low-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 80% of FeSiAl soft magnetic alloy powder (average particle diameter of 95nm available from Kjen chemical Co., ltd., shanghai) and epoxy EP-12 resin particles (available from Rihuan Water Co., ltd.).
The metal layer composite structure material is a copper foil with the thickness of 1.0mm, and is purchased from Shanghai Hongyu metal materials Co.
A preparation method of a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material comprises the following steps:
s1, each layer is respectively dried in four stages of a drying oven at the temperature of 60-70-80-110 ℃ through glue mixing for 30min, coating with a scraper at the angle of 47 degrees and the coating speed of 1m/min and slicing by 100 x 300mm to form semi-finished products of a microwave absorbing layer, a high-frequency absorbing layer and a low-frequency absorbing layer.
S2: and then the composite structure is sequentially overlapped with a metal layer composite structure from top to bottom to carry out high-temperature 90T hot-pressing and pressure-maintaining for 25min at the temperature of 150 ℃ for bonding.
The glue mixing process uses a ZH-1600 glue mixer produced by Convolvulation Automation technology Limited in Dongguan city, a 1200-type scraper coater produced by Bentai packaging machinery Limited in Longhong city is used in the coating process, and the high-temperature hot-pressing equipment uses an HBSCR- (600-2000) t hot press produced by Huabo mechanical science and technology Limited in Qingdao to perform hot pressing.
Example 2
The embodiment 2 of the invention discloses a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material which comprises the following components in parts by weight: the composite structure comprises a microwave absorbing layer, a high-frequency absorbing layer, a low-frequency absorbing layer and a metal layer composite structure from top to bottom; the wave absorbing frequency band of the microwave absorbing layer is 10GHz-40GHz, the wave absorbing frequency band of the high-frequency wave absorbing layer is 1GHz-10GHz, and the wave absorbing frequency band of the low-frequency wave absorbing layer is 100MHz-1GHz.
The microwave absorbing layer comprises the following raw materials in percentage by mass: 50% carbonyl iron powder (average particle size of 10 μm from new wuhan diamond material co., ltd.), 2% graphene powder (average particle size of 100nm from pioneer nano material technology co., ltd.), and the balance TPU resin (RH 4037 particles from new wuhan diamond material co., ltd.).
The preparation raw materials of the high-frequency wave-absorbing layer comprise, by mass: 80% by weight of FeSi65 soft magnetic alloy powder (average particle diameter of 95nm, available from Beijing Yijin New materials Co., ltd.), and the balance of thermosetting acrylic resin particles (Setalux 1762 available from Shanghai Kai Yin chemical Co., ltd.).
The low-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 90% by weight of FeSiAl soft magnetic alloy powder (average particle diameter of 95nm, available from Kjen chemical Co., ltd., shanghai) and epoxy EP-12 resin particles (available from Rikawa Kagaku Co., ltd., henan).
The metal layer composite structure material is a copper foil with the thickness of 1.0mm, and is purchased from Shanghai Hongyu metal materials Co.
A preparation method of a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material comprises the following steps:
s1, each layer is respectively dried in four stages of a drying oven at the temperature of 60-70-80-110 ℃ through glue mixing for 30min, coating with a scraper at the angle of 47 degrees and the coating speed of 1m/min and slicing by 100 x 300mm to form semi-finished products of a microwave absorbing layer, a high-frequency absorbing layer and a low-frequency absorbing layer.
S2: and then the composite structure is sequentially overlapped with a metal layer composite structure from top to bottom to carry out high-temperature 90T hot-pressing and pressure-maintaining for 25min at the temperature of 150 ℃ for bonding.
The glue mixing process uses a ZH-1600 glue mixer produced by Convolvulation Automation technology Limited in Dongguan city, a 1200-type scraper coater produced by Bentai packaging machinery Limited in Longhong city is used in the coating process, and the high-temperature hot-pressing equipment uses an HBSCR- (600-2000) t hot press produced by Huabo mechanical science and technology Limited in Qingdao to perform hot pressing.
Example 3
The embodiment 3 of the invention discloses a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material which comprises the following components in parts by weight: the composite structure comprises a microwave absorbing layer, a high-frequency absorbing layer, a low-frequency absorbing layer and a metal layer composite structure from top to bottom; the wave absorbing frequency band of the microwave absorbing layer is 10GHz-40GHz, the wave absorbing frequency band of the high-frequency wave absorbing layer is 1GHz-10GHz, and the wave absorbing frequency band of the low-frequency wave absorbing layer is 100MHz-1GHz.
The microwave absorbing layer comprises the following raw materials in percentage by mass: 40% carbonyl iron powder (average particle size of 10 μm from new Wuhan Diamond materials Co., ltd.), (1.2% graphene powder having average particle size of 100nm from pioneer nanomaterial technology Co., ltd.), (RH 4037 particles from new Wuhan Diamond materials Co., ltd.), and the balance TPU resin.
The preparation raw materials of the high-frequency wave-absorbing layer comprise, by mass: 70% of FeSi65 soft magnetic alloy powder (average particle diameter of 95nm, available from Beijing Yijin New materials Co., ltd.), and the balance of thermosetting acrylic resin particles (Setalux 1762 available from Shanghai Kai Yin chemical Co., ltd.).
The low-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 85% FeSiAl soft magnetic alloy powder) having an average particle diameter of 95nm, which was obtained from Kjeldahl chemical Co., ltd., shanghai), and epoxy EP-12 resin particles (obtained from Rikawa Kagaku Co., ltd., henan).
The metal layer composite structure material is a copper foil with the thickness of 1.0mm, and is purchased from Shanghai Hongyu metal materials Co.
A preparation method of a high-temperature-resistant soft magnetic multilayer composite wave-absorbing material comprises the following steps:
s1, each layer is respectively dried in four stages of a drying oven at the temperature of 60-70-80-110 ℃ through glue mixing for 30min, coating with a scraper at the angle of 47 degrees and the coating speed of 1m/min and slicing by 100 x 300mm to form semi-finished products of a microwave absorbing layer, a high-frequency absorbing layer and a low-frequency absorbing layer.
S2: and then the composite structure is sequentially overlapped with a metal layer composite structure from top to bottom to carry out high-temperature 90T hot-pressing and pressure-maintaining for 25min at the temperature of 150 ℃ for bonding.
The glue mixing process uses a ZH-1600 glue mixer produced by Convolvulation Automation technology Limited in Dongguan city, a 1200-type scraper coater produced by Bentai packaging machinery Limited in Longhong city is used in the coating process, and the high-temperature hot-pressing equipment uses an HBSCR- (600-2000) t hot press produced by Huabo mechanical science and technology Limited in Qingdao to perform hot pressing.
Comparative example 1
The carbonyl iron powder particle size was 20 μm, and the rest was the same as in example 2.
Comparative example 2
The particle size of the FeSi65 soft magnetic alloy powder was 50nm, and the rest was the same as in example 2.
Performance test method
1. And (3) magnetic permeability test: the composite wave-absorbing material obtained in the examples 1-3 and the comparative examples 1-2 is tested by using a magnetic permeability tester, the test method refers to GB/T35690-2017 'test method for weak magnetic relative magnetic permeability', and the measured data are recorded in Table 1.
2. And (3) conductivity testing: the composite wave-absorbing material obtained in the examples 1-3 and the comparative examples 1-2 is tested by a conductivity tester, and the test method refers to GB/T15662-1995 'test method for volume resistivity of conductive and antistatic plastics'
3. And (3) testing high-temperature performance: the composite wave-absorbing material obtained in the examples 1-3 and the comparative examples 1-2 is put into a thermal stability tester, the test method refers to GB/T3512-2014, and the measured data are recorded in Table 1.
Performance test data
TABLE 1
| Magnetic conductivity (mu) | Conductivity (omega/sq) | High temperature resistance (DEG C) | |
| Example 1 | 136.5 | 10^6 | 120 |
| Example 2 | 212.4 | 10^3 | 150 |
| Example 3 | 186.6 | 10^5 | 150 |
| Comparative example 1 | 218.7 | 10^3 | 150 |
| Comparative example 2 | 208.1 | 10^3 | 150 |
Claims (10)
1. A high temperature resistant soft magnetic composite wave-absorbing material is characterized in that: the microwave absorbing material comprises a microwave absorbing layer, a high-frequency absorbing layer, a low-frequency absorbing layer and a metal layer composite structure from top to bottom; the wave absorbing frequency band of the microwave absorbing layer is 10GHz-40GHz, the wave absorbing frequency band of the high-frequency wave absorbing layer is 1GHz-10GHz, and the wave absorbing frequency band of the low-frequency wave absorbing layer is 100MHz-1GHz.
2. The composite wave-absorbing material of claim 1, wherein: the microwave absorbing layer comprises the following raw materials in percentage by mass: 35-50% carbonyl iron powder, 1-2% graphene powder, and the balance first resin particles.
3. The composite wave-absorbing material of claim 2, wherein: the average grain diameter of the carbonyl iron powder is 1-10 mu m.
4. The composite wave-absorbing material of claim 1, wherein: the preparation raw materials of the high-frequency wave-absorbing layer comprise, by mass: 60-80% of the FeSi65 soft magnetic alloy powder, and the balance of the second resin particles.
5. The composite wave-absorbing material of claim 4, wherein: the average grain diameter of the FeSi65 soft magnetic alloy powder is 90-100 nm.
6. The composite wave-absorbing material of claim 1, which is characterized in that: the low-frequency wave-absorbing layer is prepared from the following raw materials in percentage by mass: 80-90% of FeSiAl soft magnetic alloy powder and the balance of third resin particles.
7. The composite wave-absorbing material of claim 6, which is characterized in that: the third resin particles are epoxy EP-12 particles.
8. The composite wave-absorbing material of claim 1, which is characterized in that: the metal layer composite structure material comprises one or more of copper foil, aluminum foil, conductive cloth and conductive film.
9. A method for preparing a high temperature resistant soft magnetic multilayer composite wave-absorbing material according to any one of claims 1 to 8, which is characterized in that: comprises the following steps
And S1, forming a semi-finished product by mixing and stirring resin sol and coating a release film on the microwave absorbing layer.
S2: and then the metal layer composite structure and the metal layer composite structure are sequentially overlapped together for high-temperature hot-pressing bonding.
10. The preparation method of the composite wave-absorbing material according to claim 9, characterized by comprising the following steps: the coating process is blade coating.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210989250.7A CN115842248A (en) | 2022-08-17 | 2022-08-17 | High-temperature-resistant soft magnetic composite wave-absorbing material and preparation method thereof |
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| CN202210989250.7A CN115842248A (en) | 2022-08-17 | 2022-08-17 | High-temperature-resistant soft magnetic composite wave-absorbing material and preparation method thereof |
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