CN105025695A - Broadband electromagnetic wave absorption complex with flame-retarding characteristics and manufacturing method of complex - Google Patents
Broadband electromagnetic wave absorption complex with flame-retarding characteristics and manufacturing method of complex Download PDFInfo
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- CN105025695A CN105025695A CN201510446995.9A CN201510446995A CN105025695A CN 105025695 A CN105025695 A CN 105025695A CN 201510446995 A CN201510446995 A CN 201510446995A CN 105025695 A CN105025695 A CN 105025695A
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- electromagnetic wave
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Abstract
The invention provides a broadband electromagnetic wave absorption complex with flame-retarding characteristics. The broadband electromagnetic wave absorption complex comprises a polymer main body 12 in which a plurality of Fe-based soft magnetic alloy particles are evenly distributed; the Fe-based soft magnetic alloy particles are covered with a Mg(OH)2 coating; the Fe-based soft magnetic alloy particles are spherical, square, flaky, needle-like, fibriform or in an irregular shape. The invention also provides a manufacturing method of the broadband electromagnetic wave absorption complex with the flame-retarding characteristics. The electromagnetic wave absorption complex is of a specific electromagnetic wave absorption structure, and therefore, the width of the electromagnetic wave absorption band can be increased and the flame-retarding characteristics also can be improved; in short, the electromagnetic wave absorption complex can be widely applied to the field of anti-electromagnetic interference of electronic products.
Description
Technical field
The present invention relates to a kind of wide band electromagnetic wave sorption complex and the manufacture method thereof with flame-retarding characteristic, this complex can be applicable to and needs on the electronic devices and components of electromagnetism interference.
Background technology
The application of electromagnetism interference (EMI) material suppresses one of the most cost-effective means of electromagnetic interference in electronic devices and components, and it is formed through specific processes by absorbent and polymeric binder usually.Absorbent refers to and effectively can absorb incident electromagnetic wave, and the class material by power conversion electromagnetic energy being consumed or electromagnetic wave is disappeared because of interference.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 comprises ferrite powder, metal powder and other nano material etc.They generally not only have dielectric loss but also have magnetic loss, are suitable as very much anti-EMI filter absorbing material, it is characterized in that: high magnetic permeability, high saturation magnetization and low coercive force.
Iron is the most basic magnetic element, and due to magnetic property excellence, rich reserves and cost advantage, ferrous alloy becomes one of most important wave absorbing agent.By suppressing formation and the eddy current of metallicl magnetic material closure domain, the anti-EMI filter performance of ghz band excellence can be obtained.But along with the increase of frequency, the eddy current loss that the low resistance of this kind of material causes limits its application at high frequency.Therefore, find a kind of technical scheme can expanded its electro-magnetic wave absorption frequency range and especially increase the assimilation effect of high band and seem particularly important.
On the other hand, the flame-retarding characteristic of electronic message unit is very necessary and crucial, because once breaking out of fire and the collapse causing electronic information will cause heavy losses.For absorbing material, the approach improving flame-retarding characteristic can be divided three classes: (1) carries out flame-retardant modified to wave absorbing agent; (2) design new polymer molecular structure and make it that there is essential high flame retardant; (3) fire retardant is added.Wherein, this method of the interpolation of fire retardant cost is lower and can realize fast.At present, fire retardant the most common is halogenated flame retardant, as TDE.But halogenated flame retardant exists and to have an impact this unavoidable problem to human body and environment always, cause its restriction being always subject to various countries' environmental protection instruction (as RoHS Directive 2002/95/EC specifies).Therefore, containing one of the exploitation important topic becoming industry development of the absorbing material of halogen-free type fire retardant.
Summary of the invention
The object of the present invention is to provide a kind of wide band electromagnetic wave sorption complex and the manufacture method thereof with flame-retarding characteristic, this electro-magnetic wave absorption complex adopts specific electromagnetic wave absorbing structure, the width of electro-magnetic wave absorption frequency range can either be increased, can flame-retarding characteristic be improved again, the field of electronic product electromagnetism interference can be widely used in.
The present invention has the wide band electromagnetic wave sorption complex of flame-retarding characteristic, its structure comprises three parts: (1) iron-base soft magnetic alloy particle, it can be spherical, square, sheet shape, needle-like, threadiness or other is irregularly shaped, and it is the main component causing electromagnetic wave attenuation to absorb; (2) at the high-resistance Mg of iron-base soft magnetic alloy particle surface compound one deck (OH)
2coating, its content is at 0.1wt% ~ 30wt%; (3) three is organic polymeric binder, it and Mg (OH)
2compound, makes iron-base soft magnetic alloy particle connect shaping.
Fig. 1 is the profile that the present invention has the wide band electromagnetic wave sorption complex of flame-retarding characteristic; In Fig. 1,11 is iron-base soft magnetic alloy particle, and 12 is polymer body 12, and 13 is Mg (OH)
2coating; Fig. 2 is the profile of common ferrous alloy wave-absorber; In Fig. 2,21 is iron-base soft magnetic alloy particle, and 22 is polymer body 12.Both fundamental differences are that the former metallic magnetic grain surface is coated by magnesium hydroxide layer.The resistivity of magnesium hydroxide can up to 1011 Ω/cm, and between magnetically soft alloy particle, increase suitable magnesium hydroxide coating can reduce magnetic action between particle, and increase resistance loss, this all contributes to the electro-magnetic wave absorption effect improving whole absorber.In addition, magnesium hydroxide is also a kind of filled-type fire retardant, discharges Bound moisture by during decomposes, absorbs a large amount of latent heat, reduce the surface temperature of synthetic material in flame that it fills, there is the effect suppressing polymer unwinds and cool produced fuel gas.Magnesium hydroxide (340 ~ 490 DEG C) when being heated decomposes, and the activated magnesia of generation is attached to the carrying out that combustible surface prevents again burning further.Magnesium hydroxide not only produces without any harmful substance in whole fire-retardant process, and its product decomposed can also absorb the macromolecule such as rubber, plastics while fire-retardant in a large number and to burn the pernicious gas and smog that produce, activated magnesia constantly absorbs imperfect combustion fusing residue, eliminating smog while stopping very soon from making burning, stoping molten drop, is a kind of good environmental protection inorganic fire retardant.
The iron-base soft magnetic alloy particle that the present invention adopts, its material includes but not limited to FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
The iron-base soft magnetic alloy particle that the present invention adopts, particle size D50 represents, the method for testing of D50 is laser particle size method (Malvern laser particle analyzer, model: MS2000).Its range intervals represents with [a, b], and wherein a is D50 lower limit, and b is D50 higher limit, and unit is micron.Its average grain diameter D50 is [1,500], preferably [10,300], is preferably [20,100].
The chemical composition of iron-base soft magnetic alloy particle surface covering of the present invention is Mg (OH)
2, its content, at [0.1wt%, 30wt%], preferably [1wt%, 20wt%], is preferably [5wt%, 10wt%].
The described organic polymer as bonding agent is thermoplastic polymer, include but not limited to: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, PETG, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, acrylonitrile-butadiene rubber, polysulfide, acrylonitrile-butadiene-styrene (ABS) (ABS), silicon rubber, natural rubber etc.Organic binder material is not limited to above-mentioned material, and optimal material can be selected to determine according to the difference of the embody rule occasion and manufacturing installation of inhaling ripple complex.
According to the feature of properties of materials difference with its preparation technology, the manufacture method of electro-magnetic wave absorption complex of the present invention comprises the steps: that (1) selects the kind of magnetic metal material according to practical situations, and prepares iron-base soft magnetic alloy particle according to aforementioned claim; (2) prepare the precursor solution of magnesium hydroxide, among the precursor solution of iron-base soft magnetic alloy particle input magnesium hydroxide, in water-based system, cover last layer Mg (OH) by chemical reaction to iron-base soft magnetic alloy particle
2layer.The relatively independent existence of particle of iron-base soft magnetic alloy/magnesium hydroxide composite powder, the content of magnesium hydroxide meets aforementioned claim; (3) above-mentioned powder is heat-treated at a certain temperature in high temperature furnace; (4) then the powder after heat treatment is mixed with thermoplastic polymeric binder, be preformed into sheet by one or more moulding processs; (5) finally hot-formingly complex is obtained.This suction ripple complex can with the combination such as DR tape, glue, be then attached to and need on the electronic devices and components of electromagnetism interference.
The precursor solution of magnesium hydroxide of the present invention comprises following characteristics: (1) slaine containing Mg element or compound; (2) can produce (OH)
-the aqueous environment of anion.
Solvent of the present invention is selected according to the type of binding agent, can be water, toluene, cyclohexanone, ethyl acetate, dimethylbenzene etc. or its combination of at least two kinds.
The methods such as moulding process of the present invention comprises spin coating, band is coated with, press mold coating, printing coating, blade coating, roller coating are coated on substrate, also can be the methods of mold pressing or roll extrusion.
Backing material of the present invention includes but not limited to the plastic films such as PET, PP or PE, or paper substrate, or metal forming, or the flexible material such as graphite film.Wherein, electronic applications is commonly coated in as metal material surfaces such as plastics and Cu, Al, Au, Ag such as PE, PET.
Advantage of the present invention and beneficial effect are: provide a kind of wide band electromagnetic wave sorption complex and the manufacture method thereof with flame-retarding characteristic, this electro-magnetic wave absorption complex adopts specific electromagnetic wave absorbing structure, the width of electro-magnetic wave absorption frequency range can either be increased, can flame-retarding characteristic be improved again, the field of electronic product electromagnetism interference can be widely used in.
Electro-magnetic wave absorption complex of the present invention, compared with identical weight percentage filling type wave-absorber, has wider absorption frequency range.
Electro-magnetic wave absorption complex of the present invention, flame-retarding characteristic is improved significantly (with reference to UL94 standard testing).
Accompanying drawing explanation
Fig. 1 the present invention has the profile of the wide band electromagnetic wave sorption complex of flame-retarding characteristic;
Fig. 2 is the profile of common iron-base soft magnetic alloy wave-absorber;
The scanning electron micrograph of the magnetically soft alloy particle/magnesium hydroxide compound obtained in Fig. 3 embodiment 1;
The X ray electronic energy spectrum of the electro-magnetic wave absorption complex obtained in Fig. 4 embodiment 1;
The electro-magnetic wave absorption collection of illustrative plates of the electromagnetic wave composite absorber obtained in Fig. 5 embodiment 2;
The electro-magnetic wave absorption collection of illustrative plates of the electromagnetic wave composite absorber obtained in Fig. 6 comparative example 1;
Flame retardant rating test result comparison diagram in Fig. 7 embodiment 3 and comparative example 2.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The invention provides a kind of wide band electromagnetic wave sorption complex with flame-retarding characteristic, comprise polymer body 12, be evenly equipped with some iron-base soft magnetic alloy particles in described polymer body 12, described iron-base soft magnetic alloy particle surface covers Mg (OH)
2coating;
Described iron-base soft magnetic alloy particle is spherical, square, sheet shape, needle-like, threadiness or irregularly shaped.
Described iron-base soft magnetic alloy particle comprises: FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
The dimension D of iron-base soft magnetic alloy particle
50(particle diameter corresponding when cumulative particle sizes percentile reaches 50%) is 1 ~ 500 micron, preferably 10 ~ 300 microns, is preferably 20 ~ 100 microns.
Described Mg (OH)
2coating, its content is 0.1wt% ~ 30wt%, preferably 1wt% ~ 20wt%, is preferably 5wt% ~ 10wt%.
Described polymer body 12 adopts thermoplastic polymer, comprise: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, PETG, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, acrylonitrile-butadiene rubber, polysulfide, acrylonitrile-butadiene-styrene copolymer, silicon rubber, natural rubber.
The present invention also provides the above-mentioned manufacture method with the wide band electromagnetic wave sorption complex of flame-retarding characteristic, comprises the steps:
1) cover last layer Mg (OH) first in water-based system iron-base soft magnetic alloy particle surface
2coating, obtains preliminary powder;
2) more above-mentioned powder is heat-treated at a certain temperature;
3) again the powder after heat treatment is mixed with thermoplastic polymer;
4) again by applying on substrate, the method preforming of mold pressing or roll extrusion;
5) finally hot-forming, obtain complex.
Described water-based system is: the slaine containing Mg element or compound, and can produce (OH)
-the aqueous environment of anion.
Described heat treatment: carry out in inert atmosphere or reducing atmosphere; Heat treatment temperature is 200 ~ 1000 DEG C, preferably 400 ~ 700 DEG C, is preferably 500 ~ 600 DEG C.
Described substrate is PET, PP or PE plastic film, or paper substrate, or metal forming, or graphite film.
Described coating comprises: spin coating, band are coated with, press mold applies, print coating, blade coating, roller coating.
The technical scheme that the present invention specifically implements is:
Embodiment 1
With Fe powder and Si powder (purity 99.9%) for original material prepares the strand of FeSi alloy, after utilizing the method for Mechanical Crushing to carry out coarse crushing to it, carry out grinding processing with sand mill.By the particle diameter D50 obtained be forerunner's magnesium hydroxide that the FeSi alloy powder 1.2 kilograms of 56 microns is put into precursor solution among, slowly stir at 60 c and take out afterwards for 2 hours, the dissociated ion of washing removing excess surface, at 180 DEG C, vacuum heat can obtain coated Mg (OH) afterwards
2feSi powder.Wherein, the precursor solution of magnesium hydroxide obtains in the following ways.Detailed process: precise 270 grams of NH4Cl add 1900 milliliters of NH
3h
2in O, be then settled to 5000 milliliters with distilled water, be mixed with the NH that pH value is 10.8
3h
2o-NH
4cl buffer solution is for subsequent use.The magnesium sulfate (analyzing pure) taking 300 grams is dissolved in the NH of 5000 milliliters
3h
2o-NH
4(produce without precipitation under normal temperature) among Cl buffer solution, namely obtain magnesium hydroxide precursor solution.To thus obtained FeSi/Mg (OH)
2powder is scanning electron Micro-Structure Analysis (SEM; INSTRUMENT MODEL: Japanese JEOL JSM-6700F) and constituent analysis (EDS; Oxford company of Britain), result is respectively as shown in Figure 3 and Figure 4.The existence at Fe, Si, Mg and O element character pair peak as seen from the figure, shows there is Mg (OH)
2the generation of material, and the surface being coated on FeSi alloying pellet.
The preparation of inhaling ripple complex mixes according to following part by weight.
FeSi/Mg (OH)
2composite powder: 80 weight portions
Toluene: 40 weight portions
Polyvinyl butyral resin: 8 weight portions
The slurry obtained is prepared in the PET film of 100 micron thickness by coating method, through 60 DEG C of heating removing toluene, is obtaining the electro-magnetic wave absorption complex that required thickness is 0.2 millimeter afterwards through hot pressing.The flame retardant rating adopting the flame retardant rating design code evaluation of UL94 to go out this complex is V1.
Embodiment 2
With Fe powder, Ni powder and Mo powder (purity 99.9%) for original material prepares the strand of molybdenum permalloy, after utilizing the method for Mechanical Crushing to carry out coarse crushing to it, carry out grinding processing with sand mill.By the particle diameter D50 obtained be forerunner's magnesium hydroxide that the molypermalloy powder 1.2 kilograms of 21 microns is put into precursor solution among, slowly stir at 60 c and take out afterwards for 2 hours, the dissociated ion of washing removing excess surface, at 180 DEG C, vacuum heat can obtain coated Mg (OH) afterwards
2feNiMo powder.Wherein, the precursor solution of magnesium hydroxide obtains in the following ways.Detailed process: precise 270 grams of NH4Cl add 1900 milliliters of NH
3h
2in O, be then settled to 5000 milliliters with distilled water, be mixed with the NH that pH value is 10.8
3h
2o-NH
4cl buffer solution is for subsequent use.The magnesium sulfate (analyzing pure) taking 300 grams is dissolved in the NH of 5000 milliliters
3h
2o-NH
4(produce without precipitation under normal temperature) among Cl buffer solution, namely obtain magnesium hydroxide precursor solution.
The preparation of inhaling ripple complex adopts mixing method to mix according to following part by weight.
FeNiMo/Mg (OH)
2composite powder: 80 weight portions
Polyvinyl chloride: 20 weight portions
The material be mixed to get is obtained through mill the electro-magnetic wave absorption complex that required thickness is 2.0 millimeters.Fig. 5 is the electro-magnetic wave absorption collection of illustrative plates (network vector analyzer, Agilent E8364A) of obtained electromagnetic wave composite absorber.
Comparative example 1
Mg (OH) is illustrated in order to contrast
2ripple material is inhaled to iron-based soft magnetic and can play the effect of expanding and absorbing frequency range wide cut, prepared comparative example 1 sample: the preparation of molybdenum permalloy particle is identical with embodiment 2, but without Mg (OH)
2coated process.The preparation method inhaling ripple complex describes with embodiment 2.Molypermalloy powder in formula: 80 weight portions, polyvinyl chloride: 20 weight portions.Fig. 6 is the electro-magnetic wave absorption collection of illustrative plates (Agilent network vector analyzer, model: E8364A) of obtained electromagnetic wave composite absorber.As can be seen from Fig., two kinds of suction ripple complexs have obvious absorption to electromagnetic wave.Compared with Fig. 5, the absorption region in Fig. 6 increases to some extent, is embodied directly in absorb minimum and obtain position and change to 2.57GHz by 2.12GHz, and the dB value simultaneously during 10GHz changes to-4.66 by-3.55.As can be seen here, Mg (OH)
2the wide cut adding the absorption frequency range having widened electromagnetic wave absorbent material.
Embodiment 3
With Fe powder and Ni powder (purity 99.9%) for original material prepares the strand of FeNi48 alloy, after utilizing the method for Mechanical Crushing to carry out coarse crushing to it, carry out grinding processing with sand mill.By the particle diameter D50 obtained be forerunner's magnesium hydroxide that the FeNi alloy powder 0.8 kilogram of 47 microns is put into precursor solution among, slowly stir at 60 c and take out afterwards for 2 hours, the dissociated ion of washing removing excess surface, at 180 DEG C, vacuum heat can obtain coated Mg (OH) afterwards
2feNi48 powder.Wherein, the precursor solution of magnesium hydroxide obtains in the following ways.Detailed process: precise 270 grams of NH
4cl adds 1900 milliliters of NH
3h
2in O, be then settled to 5000 milliliters with distilled water, be mixed with the NH that pH value is 10.8
3h
2o-NH
4cl buffer solution is for subsequent use.The magnesium sulfate (analyzing pure) taking certain gram is dissolved in the NH of 5000 milliliters
3h
2o-NH
4(produce without precipitation under normal temperature) among Cl buffer solution, namely obtain magnesium hydroxide precursor solution.The consumption changing magnesium sulfate can obtain Mg (OH)
2the composite granule that content is different.
The preparation of inhaling ripple complex mixes according to following part by weight.
FeNi/Mg (OH)
2composite powder: 80 weight portions, wherein Mg (OH)
2content be A sample 5wt%, B sample 10wt%, C sample 15wt%.
Ethylene propylene rubber: 8 weight portions
By the powder obtained by banburying with open the method for refining and ethylene propylene rubber mixes, be then molded into sheet and obtain the electro-magnetic wave absorption complex that required thickness is 0.5 millimeter.The flame retardant rating design code evaluation of UL94 is adopted to go out different Mg (OH)
2the flame-retarding characteristic of the complex of content.
Comparative example 2
In order to Mg (OH) is described
2and content is on the impact of electro-magnetic wave absorption complex fire resistance, preparation is not containing the suction ripple material sample of any fire retardant, and process is with embodiment 3.Adopt the method for UL94 plastic flame grade to carry out sign fire resistance, after carrying out twice combustion testings of 10 seconds by observation to sample, the time of fray-out of flame evaluates its quality, and result as shown in Figure 7.As seen from the figure, Mg (OH)
2after the introducing of composition, the time of fray-out of flame obviously shortens, and content is larger, and the time of fray-out of flame is shorter, shows that flame-retarding characteristic is progressively improving.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. there is the wide band electromagnetic wave sorption complex of flame-retarding characteristic, it is characterized in that:
Comprise polymer body 12, be evenly equipped with some iron-base soft magnetic alloy particles in described polymer body 12, described iron-base soft magnetic alloy particle surface covers Mg (OH)
2coating;
Described iron-base soft magnetic alloy particle is spherical, square, sheet shape, needle-like, threadiness or irregularly shaped.
2. the wide band electromagnetic wave sorption complex with flame-retarding characteristic according to claim 1, is characterized in that, described iron-base soft magnetic alloy particle comprises: FeSi, FeAl, FeSiAl, FeSiB, FeNi, FeCo.
3. the wide band electromagnetic wave sorption complex with flame-retarding characteristic according to claim 2, is characterized in that, the dimension D of iron-base soft magnetic alloy particle
50be 1 ~ 500 micron, preferably 10 ~ 300 microns, be preferably 20 ~ 100 microns.
4. the wide band electromagnetic wave sorption complex with flame-retarding characteristic according to claim 3, is characterized in that, described Mg (OH)
2coating, its content is 0.1wt% ~ 30wt%.
5. the wide band electromagnetic wave sorption complex with flame-retarding characteristic according to claim 4, it is characterized in that, described polymer body 12 adopts thermoplastic polymer, comprise: polyester resin, polyvinyl resin, Corvic, polypropylene, polystyrene, Merlon, nylon, epoxy resin, polyacrylics, polyurethane resin, polyvinyl butyral resin, PETG, polybutylene terephthalate (PBT), fiber-like resin, itrile group butadiene type rubber, styrene butadiene class rubber, butyl rubber, chlorinated polyethylene rubber, ethylene propylene rubber, acrylonitrile-butadiene rubber, polysulfide, acrylonitrile-butadiene-styrene copolymer, silicon rubber, natural rubber.
6. there is according to any one of claim 1-5 the manufacture method of the wide band electromagnetic wave sorption complex of flame-retarding characteristic, comprise the steps:
1) cover last layer Mg (OH) first in water-based system iron-base soft magnetic alloy particle surface
2coating, obtains preliminary powder;
2) more above-mentioned powder is heat-treated at a certain temperature;
3) again the powder after heat treatment is mixed with thermoplastic polymer;
4) again by applying on substrate, the method preforming of mold pressing or roll extrusion;
5) finally hot-forming, obtain complex.
7. the manufacture method with the wide band electromagnetic wave sorption complex of flame-retarding characteristic according to claim 6, it is characterized in that, described water-based system is: the slaine containing Mg element or compound, and can produce (OH)
-the aqueous environment of anion.
8. the manufacture method with the wide band electromagnetic wave sorption complex of flame-retarding characteristic according to claim 7, is characterized in that, described heat treatment: carry out in inert atmosphere or reducing atmosphere; Heat treatment temperature is 200 ~ 1000 DEG C.
9. the manufacture method with the wide band electromagnetic wave sorption complex of flame-retarding characteristic according to claim 8, is characterized in that, described substrate is PET, PP or PE plastic film, or paper substrate, or metal forming, or graphite film.
10. the manufacture method with the wide band electromagnetic wave sorption complex of flame-retarding characteristic according to claim 9, it is characterized in that, described coating comprises: spin coating, band are coated with, press mold applies, print coating, blade coating, roller coating.
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