CN105992508A - Novel nanostructure electromagnetic wave absorption complex and manufacturing method thereof - Google Patents
Novel nanostructure electromagnetic wave absorption complex and manufacturing method thereof Download PDFInfo
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Abstract
A novel nanostructure electromagnetic wave absorption complex is characterized in that (1) electromagnetic wave absorbents are distributed in a continuous polymer layer; (2) the distances between the electromagnetic wave absorbents and the distribution of the electromagnetic wave absorbents in the polymer layer are in regular arrangement according to the used masks; (3) the electromagnetic wave absorbents are uniformly regular circular or square sheets, and the plane size of each sheet of electromagnetic wave absorbent is within 500 micrometers; (4) the area sum of all electromagnetic wave absorbents is greater than the plane area of the electromagnetic wave absorption complex in an incident direction. The novel nanostructure electromagnetic wave absorption complex of the present invention can solve the electrostatic capacitance problem of an alternatively laminated structure, at the same time, does not depend on the flat metal powder, has a high magnetic conductivity, and can be widely used in the electronic product anti-electromagnetic interference field.
Description
Technical field
The present invention relates to a kind of novel nano structure electro-magnetic wave absorption complex, the electronic devices and components need electromagnetism interference have wide practical use.The invention still further relates to obtain the manufacture method of this novel nano structure electro-magnetic wave absorption complex.
Background technology
The high frequency of electronic equipment is the inexorable trend of market development, and this makes the electromagnetic interference (EMI) produced between electronic devices and components accordingly increase, thus has influence on the normal work of equipment.Meanwhile, people are to healthy more concern, it is to avoid the demand of unnecessary electromagnetic radiation also promotes the development of electromagnetism interference technology.Anti-EMI material is one of the most cost-effective means of suppression electromagnetic interference, and it is generally made up of absorbent and binding agent.Absorbent refers to effectively absorb incident electromagnetic wave, and is changed class material electromagnetic energy being consumed or making electromagnetic wave disappear because of interference by energy.According to the difference of absorption mechanism, the lossy medium of absorbing material can be divided into resistor-type, dielectric type and magnetizing mediums type three class.
Magnetic loss material includes ferrite powder, super-fine metal powder and other nano material etc..They the most not only have dielectric loss but also have magnetic loss, are highly suitable as anti-EMI filter absorbing material, it is characterized in that: high pcrmeability, high saturation magnetization and low coercivity.At present, study and apply more ripe is ferrite series absorbing material, the whole market of Antl-GBM nephritis occupies leading position.Although Ferrite Material has good stability, but due to the restriction of the Snoke limit, when absorbing the clutter of microwave frequency band, volume is too big, and frequency band absorbs the widest.Compared with ferrite, the magnetic of metallicl magnetic material derives from ferromagnetic interelectric exchange-coupling interaction, and its saturation magnetization is 2-3 times of ferrite magnetic material, and Curie temperature is high, thus the electromangnetic spectrum being more suitable in high frequency environment.
Ferrum is most basic magnetic element, and due to magnetic property excellence, rich reserves and cost advantage, ferrous alloy becomes one of most important metal soft magnetic material.But being as the increase of frequency, the eddy-current loss that the low resistance of conventional soft magnetic materials is caused limits its application at high frequency.If able to the formation of suppression metallicl magnetic material closure domain and eddy current, it is possible to obtain the anti-EMI filter performance that ghz band is more excellent than Ferrite Material.Thin magnetic film and thin dielectric film, owing to being affected by skin depth, are formed alternate laminated structure by people by the thickness of metallic film magnetic material.It is demonstrated experimentally that this structure is effective to suppression eddy current and elimination closure domain.But this structure exists electrostatic capacitance and causes the generation of displacement current, have impact on the high frequency pcrmeability of this structure.Later it has been found that the electrostatic capacitance of magnetic metal/electrolyte alternate laminated structure generation, depending on the lengthwise dimension of magnetic metal, if alternate laminated structure is divided into column, electrostatic capacitance can be ignored.Under the inspiration of this thought into, the metal part of alternate laminated structure is changed the flat powder with big aspect ratio, isolate with polymer between powder, the anti-EMI material that high frequency characteristics is excellent can be prepared.But, in actual industrial production, the performance of this kind of method is limited by flat metal powder completely, and the production efficiency of the iron-base soft magnetic alloy powder body that thickness has high aspect ratio less than 100 nanometers is the lowest, this is just unfavorable for that batch micro operations has the anti-EMI filter high frequency absorbing material of good production economy benefit.Therefore, finding one and i.e. can solve the problem that alternate laminated structure electrostatic capacitance problem, the technical scheme simultaneously not relying on again flat iron(-)base powder is particularly important.
Summary of the invention
The object of the invention is to produce a kind of novel nano structure electro-magnetic wave absorption complex, general this type of is inhaled ripple film and is mainly carried out electromagnetic wave absorption by the way of magnetic loss, according to the difference of magnetic-particle composition kind, the electromagnetic wave of different frequency scope is produced absorption, and the effect absorbed changes along with thickness and the packing ratio of thin film.Under the trend of slimming design, little and good absorbing effect the material of thickness is favored beyond doubt, and under identical weight premise, electromagnetic absorption agent thickness is the thinnest, and the number of sheet-like particle is the most, and the absorption to electromagnetic wave is the most favourable.In fact, when Metal Flake granule thickness more than its become husband's degree of depth when, unnecessary thickness to absorb be not intended to, be easily generated eddy current on the contrary.Therefore, the novel nano structure electro-magnetic wave absorption complex that the present invention provides, alternate laminated structure electrostatic capacitance problem can either be solved, do not rely on again flat metal dust simultaneously, there is preferable economic benefit, and there is high pcrmeability, can be widely applied to the field of electronic product electromagnetism interference.
The novel nano structure electro-magnetic wave absorption complex that the present invention manufactures, comprising:
(1) radio-radar absorber is distributed among continuous print polymeric layer, and radio-radar absorber is distributed among continuous print polymeric media with laminated construction, is allowed to have excellent pliability；
(2) distance between radio-radar absorber and the distribution in polymeric layer thereof are regularly arranged according to the mask used by system；
(3) radio-radar absorber is unified circle or the rule lamellar such as square, and every electromagnetic wave absorbent planar dimension is within 500 microns；
(4) the area summation of all radio-radar absorbers is amassed more than electro-magnetic wave absorption complex incident direction plane, at least ensure that radio-radar absorber covers all the polymeric layer on electromagnetic wave incident direction, in order to reach above-mentioned requirements, the radio-radar absorber of every lamination is as far as possible with the form heap row discharge staggered, to reach to use a small amount of number of plies can obtain excellent shield effectiveness.
Preferably, radio-radar absorber of the present invention is the ultra-thin iron-base soft magnetic alloy of lamination, and its composition includes FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
Preferably, ultra-thin iron-base soft magnetic alloy thickness of the present invention is preferably 5nm ~ 100 nm, more preferably 10 nm ~ 100 nm, most preferably 50 nm ~ 100 nm.
Preferably, the layer number of ultra-thin iron-base soft magnetic alloy of the present invention is more than 2 layers.
Preferably, polymeric layer of the present invention is selected from one of following: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, polyethylene terephthalate, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, nitrile rubber, polysulfide, silicone rubber, natural rubber.
According to the different feature with its preparation technology of the characteristic of every layer material, the manufacture method of novel nano structure electro-magnetic wave absorption complex of the present invention uses order below: (1) prepares the backing material of certain size, it is desirable to its material has the feature of flexibility；(2) on substrate, it is coated with last layer continuous print and there is the polymeric film of certain bonding characteristic, and remove solvent；(3) mask with holes covered above polymeric film and be adjacent to；(4) entirety obtained in step (3) is put in the chamber of physical vapour deposition (PVD), chamber is prepared with the soft magnetic metal source that will deposit；(5) carry out plated film in the chamber, porose position deposits ultra-thin iron-base soft magnetic alloy thin layer；(6) remove mask, coat the adhesive polymeric film of the second layer on surface, both covered the ultra-thin iron-base soft magnetic alloy of preceding layer, filled and led up again ultra-thin iron-base soft magnetic alloy interlayer sinking plane；(7) repeating steps 3-6 suddenly, the placement of each mask can not be completely overlapped, until the polymeric layer on electromagnetic wave incident direction is completely covered；(8) complex is placed in the environment of hot pressing, prevents from peeling off increasing the adhesion strength of thin metal layer and polymeric binder.
Backing material of the present invention includes the flexible materials such as the plastic foils such as PET, PP or PE, or paper substrate, or metal forming, or graphite film.
Polymeric layer of the present invention is thermoplastic polymer, including: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, polyethylene terephthalate, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, nitrile rubber, polysulfide, silicone rubber, natural rubber etc..But, optimal material to select to determine according to the difference of the particular use of laminated film and manufacture device.
The rule external forms such as mask of the present invention has the feature that on (1) mask and is dispersed with series of micropores, and hole is square, circular；(2) in hole, side is preferred between 1 μm ~ 500 μm to opposite side distance, more preferably 10 μm ~ 300 μm, most preferably 50 ~ 200 μm.
Described ultra-thin iron-base soft magnetic alloy, its composition includes FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
Polymeric binder of the present invention can mix with the solvent of water, toluene, Ketohexamethylene, hexamethylene, ethyl acetate, dimethylbenzene etc. or the combination of its at least two, uses the mode film forming such as roller coat, blade coating, spin coating or spraying afterwards.
Physical gas-phase deposite method of the present invention includes the methods such as electron beam evaporation, pulsed laser deposition, magnetron sputtering plating, ion film plating, thermal evaporation, the method that preferably need not substrate carries out more than 200 degrees Celsius heating.
The novel nano structure electro-magnetic wave absorption complex being made up of four-layer structure of the present invention will be further elucidated with below by specific embodiments and the drawings.
Accompanying drawing explanation
Fig. 1 by embodiment 1 the shape facility figure of employing square micropore mask;
Fig. 2 is the preparation flow figure of novel nano structure electro-magnetic wave absorption complex in embodiment 1；
Fig. 3 is the outward appearance pictorial diagram of the novel nano structure electro-magnetic wave absorption complex obtained in embodiment 1；
Fig. 4 by embodiment 2 the outline plan figure of the circular micropore mask of employing；
Fig. 5 is the magnetic property collection of illustrative plates of the novel nano structure electro-magnetic wave absorption complex obtained in embodiment 2；
Fig. 6 is the magnetic property collection of illustrative plates of the electro-magnetic wave absorption complex of the identical weight absorbent that common fill process obtains in comparative example 1.
Specific embodiment
Embodiment 1
(1) preparing a diameter of 60 mm thickness is that the PET transparent material 11 of 75 microns is as base material；(2) selecting model is that the acrylic acid glue of DP810 is as binding agent, PET is coated with the polypropylene sorrel 12(spin coater of the thick band caking property of last layer 5 microns by the method for spin coating and uses the spin coater of Laurell company of U.S. WS-400B-6NPP-LITE type), and be dried and remove solvent；(3) the band aperture mask 13 that material is politef being covered above polymeric film and is adjacent to, the shape facility of mask is as shown in Figure 1.Having uniform square hole to be distributed in circular masks, square hole arranges with box formation, and the length of side is 200 microns, and sideline spacing is 200 microns；PET/ polyacrylic acid glued membrane/microporous teflon membran (such as Fig. 2 c) is placed and is fixed in magnetron sputtering coater (JGP type rf magnetron sputtering instrument prepared by Shenyang scientific instrument limited company)；(4) with FeSi6.5Alloy is target, and sputtering power is 100 W, Ar throughput 30 sccm, and sputtering pressure is 2 Pa, and temperature is 150oOccurring deposition to obtain thickness on PET/ polyacrylic acid glued membrane/microporous teflon membran top layer under conditions of C and time 7 min is 70 nanometer Fe Si thin layers 14；(5) poly tetrafluoroethylene of release band micropore, exposes the FeSi thin metal layer of 70 nanometer thickness, and before repeating, second step obtains Fig. 2 f；(6) again microporous teflon membran is affixed on top, it is noted that 100 microns (such as Fig. 2 g) that the position of this 200 micrometer Millipore and previous micro well locations misplaced；(7) repeat front 4th step and again obtain the FeSi thin layer (such as Fig. 2 h) of new one layer of 70 nanometer thickness；(8) repeat the 5th ~ 7 step 8 time, the electromagnetic wave composite absorber (such as Fig. 2 j) that the polypropylene acid layer on electromagnetic wave incident direction is completely covered can be obtained；(9) complex is placed in the environment of hot pressing, with 120oThe condition compacting of C and 10 MPa pressure makes the adhesion strength between each lamination and between FeSi thin layer and polyacrylic acid binding agent be improved.The outward appearance pictorial diagram of the novel nano structure electro-magnetic wave absorption complex prepared is as it is shown on figure 3, material has good pliability, outward appearance gray.
Embodiment 2
(1) preparing a diameter of 100 mm thickness is that the PP transparent material of 75 microns is as base material；(2) select polrvinyl chloride as binding agent, PP is coated with 10 microns of thick polychloroethylene films of the last layer spin coater of Laurell company of U.S. WS-400B-6NPP-LITE type (spin coater use) by the method for spin coating, and be dried and remove solvent xylene；(3) the band aperture mask 13 that material is politef being covered above polymeric film and is adjacent to, the shape facility of mask is as shown in Figure 4.Having uniform circular hole to be distributed in circular masks, circular hole arranges with box formation, and a diameter of 100 microns, center of circle spacing is 150 microns；PP/ polychloroethylene film/microporous teflon membran is placed and is fixed in electron beam evaporation deposition machine (moral instrument DE600 electronic beam evaporation vacuum coating system)；(4) with FeNi48Alloy block is source, vacuum: 2.6 × 10-4Pa, evaporation rate: 20 ~ 25 A/s, substrate temperature: 120oC；Steam away from 45cm；Evaporation time: 40 min；Electron gun voltage: 9KV；Electron gun current: occurring deposition to obtain thickness on PET/ polyacrylic acid glued membrane/microporous teflon membran top layer under conditions of 0.2A is 90 nanometer Fe Ni48Alloy thin layer；(5) poly tetrafluoroethylene of release band micropore, repeats gluing-coating process 20 times, and microporous teflon membran the most all offsets in the range of 1 mm, to obtain the electromagnetic wave composite absorber that the polyvinyl chloride layer on electromagnetic wave incident direction is completely covered；(6) complex is placed in the environment of hot pressing, with 80oThe condition compacting of C and 10 MPa pressure makes between each lamination and FeNi48Adhesion strength between alloy thin layer and polrvinyl chloride is improved.The method using thermal weight loss measures FeNi in the present embodiment sample48The percentage by weight of alloy thin layer is 85.34%.
Fig. 5 is the magnetic property collection of illustrative plates (using Agilent 4991A electric impedance analyzer to measure) of novel nano structure electro-magnetic wave absorption complex obtained in embodiment 2.As seen from the figure, pcrmeability real part is on a declining curve along with the increase of frequency, and the pcrmeability of 10 MHz reaches 85.6.
Comparative example 1
For obtaining the FeNi of percentage by weight same as in Example 248Alloying pellet filled-type electro-magnetic wave absorption complex, weighs 300 grams of FeNi48Alloy, uses ball-milling technology (material: ball: ethanol=1: 12: 5, rotating speed 500 r/min) that alloying pellet is crushed to fine grained (D10=29.01 m, D50=66.63 m, D90=108.02 m).Take xylene solution mixing (solid content of polrvinyl chloride is 14.66%) of 256 grams of these alloyed powders and 300 grams of polrvinyl chloride after drying, use the method for blade coating to obtain 120 microns of thick filled-type electro-magnetic wave absorption complexs.
Fig. 6 is the magnetic property collection of illustrative plates of electro-magnetic wave absorption complex in this comparative example, and pcrmeability real part during 10 MHz is 21.1.Relatively can draw compared with Fig. 5, under conditions of same absorbent agent usage amount, the novel nano structure electro-magnetic wave absorption complex that the present invention is constructed has higher pcrmeability, and the pcrmeability of 10 MHz in Fig. 5 is 4.05 times of the pcrmeability of 10 MHz in Fig. 6.
Present invention is primarily based on as above preferred implementation to explain.But, the present invention can be by the degree of those skilled in the art's suitable change or correction invention scope.As long as these variations are without departing substantially from idea of the invention, it is clear that it is in the range of right of the present invention.
Claims (8)
1. a novel nano structure electro-magnetic wave absorption complex, it is characterised in that:
(1) radio-radar absorber is distributed among continuous print polymeric layer；(2) distance between radio-radar absorber and the distribution in polymeric layer thereof are regularly arranged according to the mask used by system；(3) radio-radar absorber is unified circle or the rule lamellar such as square, and every electromagnetic wave absorbent planar dimension is within 500 microns；(4) the area summation of all radio-radar absorbers is amassed more than electro-magnetic wave absorption complex incident direction plane.
Novel nano structure electro-magnetic wave absorption complex the most according to claim 1, it is characterised in that described radio-radar absorber is the ultra-thin iron-base soft magnetic alloy of lamination, and its composition includes FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
Novel nano structure electro-magnetic wave absorption complex the most according to claim 2, it is characterised in that described ultra-thin iron-base soft magnetic alloy thickness is preferably 5nm ~ 100 nm, more preferably 10 nm ~ 100 nm, most preferably 50 nm ~ 100 nm.
Novel nano structure electro-magnetic wave absorption complex the most according to claim 3, it is characterised in that the layer number of described ultra-thin iron-base soft magnetic alloy is more than 2 layers.
Novel nano structure electro-magnetic wave absorption complex the most according to claim 1, it is characterized in that told polymeric layer is selected from one of following: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, polyethylene terephthalate, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, nitrile rubber, polysulfide, silicone rubber, natural rubber.
6. the method preparing novel nano structure electro-magnetic wave absorption complex, the method comprises the following steps:
(1) substrate of certain size is prepared, it is desirable to its material has the feature of flexibility；(2) on substrate, it is coated with last layer continuous print and there is the polymeric film of certain bonding characteristic, and remove solvent；(3) mask with holes covered above polymeric film and be adjacent to；(4) entirety that step (3) obtains is put in the chamber of physical vapour deposition (PVD), chamber is prepared with the soft magnetic metal source that will deposit；(5) carry out plated film in the chamber, porose position deposits ultra-thin iron-base soft magnetic alloy thin layer；(6) remove mask, coat the adhesive polymeric film of the second layer on surface, both covered preceding layer ultra-thin iron-base soft magnetic alloy thin layer, and filled and led up again sinking plane between ultra-thin iron-base soft magnetic alloy thin layer；(7) repeating steps 3-6 suddenly, the placement of each mask can not be completely overlapped, until the polymeric layer on electromagnetic wave incident direction is completely covered by ultra-thin iron-base soft magnetic alloy；(8) complex that step (7) obtains is placed in the environment of hot pressing, prevents from peeling off increasing the adhesion strength of ultra-thin iron-base soft magnetic alloy layer and polymeric layer.
Method the most according to claim 5, wherein said mask has the feature that on (1) mask and is dispersed with in unified circle or the hole of the rule external form such as square；(2) in hole, side is preferred between 1 μm ~ 500 μm to opposite side distance, more preferably 10 μm ~ 300 μm, most preferably 50 ~ 200 μm.
Method the most according to claim 5, wherein said physical vapour deposition (PVD) includes electron beam evaporation, pulsed laser deposition, magnetron sputtering plating, ion film plating, thermal evaporation, the method that preferably need not substrate carries out more than 200 degrees Celsius heating.
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