CN105273689A - Novel multi-element structure composite conductive filling material - Google Patents
Novel multi-element structure composite conductive filling material Download PDFInfo
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- CN105273689A CN105273689A CN201410693341.1A CN201410693341A CN105273689A CN 105273689 A CN105273689 A CN 105273689A CN 201410693341 A CN201410693341 A CN 201410693341A CN 105273689 A CN105273689 A CN 105273689A
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Abstract
The invention discloses a multi-element structure composite conductive filling material. A surface of lightweight inorganic powder (hollow glass beads, mica, carbon fibers, flake graphite and the like) is plated with a layer of wave absorbing magnetic material (Ni, Fe, Co, Ni-P, Co-P, Ni-Co-P, Co-W-P, barium ferrite, ferriferrous oxide, carbonyl iron and the like), and then is plated with a layer of conductive material (such as metal of silver, nickel, copper and the like or inorganic oxides of doped tin oxide, doped indium oxide, doped zinc oxide, titanium dioxide and the like), and a novel multi-element structure composite conductive filling material-inorganic powder core/magnetic material coating layer/conductive material coating layer is prepared. The electromagnetic shielding performance of the composite conductive filling materials can be raised further by utilization of wave absorbing performances of the wave absorbing material to electromagnetic waves and the reflection performances of the conductive material to electromagnetic waves. The composite conductive filling material has advantages of light weight, low cost, wide shield frequency band, good shielding properties and the like, and has great application values in the electromagnetic shielding composite material field.
Description
Technical field
The invention belongs to field of functional materials, relate to a kind of multi-factor structure complex conductive fillers.The magneticsubstance of ripple is inhaled at inorganic powder surface plating one deck, plating layer of conductive material again, obtained new multicomponent structure composite conductive filler material-inorganic powder kernel/magneticsubstance coating/electro-conductive material coating, it has, and quality is light, cost is low, advantage such as shielding bandwidth, advantages of good shielding performance etc., can be used for electromagnetic shielding composite material field.
Background technology
Along with developing rapidly of the science and technology such as radar, microwave communication and electronic countermeasure, electromagnetic interference (EMI) problem is on the rise, for realizing electromagnetic wave proof, electromagnetic shielding material development rapidly, and is more and more subject to the attention of vast investigation of materials worker.Electromagnetic shielding material is based on filled-type electromagnetic shielding composite material, it has the advantage that cost is low, construction technology simple, can construct to various complicated shape, be subject to extensive concern, mainly use filled-type electromagnetic shielding composite material to carry out electromagnetic protection at present in the world.
Shielding filler is the important primitive of filled-type electromagnetic shielding composite material, is the key point affecting Materials ' Shielding Effectiveness and various application performance quality.Current shielding filler mainly contains: (1) metallic conductive fillers: the mainly metallic conductive fillers such as silver, copper and mickel; Silver, copper, electric conductivity large, effectiveness is good, but Ag price; In addition Cu is oxidizable and reduce electroconductibility, therefore must carry out special anti-oxidation process; Though nickel has certain magnetic property, chemical stability is better, but electric conductivity is lower than Cu and Ag, therefore shield effectiveness is not as the former.(2) metal inhales ripple filler: conventional metal inhales ripple filler Z 250, magneticmetal micro mist (carbonyl iron dust, iron-cobalt-nickel and alloy thereof), polycrystalline iron fiber etc., but this metalloid suction ripple filler also exists the shortcomings such as density is large, hot properties is poor.(3) Core-shell Composite Particles such as silver-coated copper powder or silver coated nickel powder, when their major advantage is to keep high conductivity, improves the cost performance of filler.Extraordinary conducting polymer composite also has good application prospect in electromagnetic shielding field, but also there is the problems such as cost height and poor electric conductivity simultaneously.
Above-mentioned metal electromagnetic shielding filler disadvantage is in the application that density is large, easily sedimentation from formed substrates, precipitation, and is difficult to the requirement meeting modern electronic product " gently ".In order to make up the defect of above-mentioned filler, Chinese scholars is with inexpensive, the material of light weight is (as glass, mica, graphite, carbon fiber etc.) as substrate or core, its Surface coating one deck or which floor chemical stability good, rotproofness is strong, the high conducting material of specific conductivity is (as silver, nickel, the metals such as copper or doped stannum oxide, doped indium oxide, doping zinc-oxide, the inorganic oxides such as titanium dioxide) or the good absorbing material (Ni of absorbing property, Fe, Co, Ni-P, Co-P, Ni-Co-P, Co-W-P, barium ferrite, Z 250, iron carbonyl etc.), make its surface metalation and obtain the nonmetal shielding filler of metallic cover.The type shielding filler features such as high or absorbing property is good with its light weight, stable physical property, specific conductivity have application prospect very widely.
Reflection loss and absorption loss being combined is one of the emphasis direction of electromagnetic shielding material research, as: adopt MULTILAYER COMPOSITE/multiple filler compounding technology to give conduction and the magnetic property of electromagnetic shielding composite material, thus improve the electromagnet shield effect of material, but create the problems such as the thickness of material increases and complete processing is complicated simultaneously.Silver-plated magnetic powder is a kind of novel electromagnetic shielding complex conductive fillers, it utilizes magneticsubstance to improve the capability of electromagnetic shielding of composite electromagnetic shield materials to electromagnetic absorptive character and electro-conductive material further to electromagnetic reflecting properties, and research shows that the coating for EMI shielding material adopting silver-plated magnetic powder to prepare has excellent effectiveness of shielding.A wider range of this type of electromagnetic shielding complex conductive fillers shielding electromagnetic wave, it will have very large using value in electromagnetic shielding field.
Summary of the invention
The object of this invention is to provide a kind of multi-factor structure complex conductive fillers, its specific descriptions are as follows:
The magneticsubstance of ripple is inhaled at inorganic powder surface plating one deck, then plating layer of conductive material, obtained new multicomponent structure composite conductive filler material-inorganic powder kernel/magneticsubstance coating/electro-conductive material coating.
Above-mentioned inorganic powder kernel is the inorganic materials of the light weights such as hollow glass micropearl, mica, carbon fiber, flake graphite, carbon nanotube, glass fibre.
Above-mentioned magneticsubstance is Ni, Fe, Co, Cr, Nd, Mo, Ni-P, Co-P, Ni-Co-P, Co-W-P, barium ferrite, Z 250, iron carbonyl etc.
Above-mentioned electro-conductive material is the metals such as silver, nickel, copper or the inorganic oxide such as doped stannum oxide (as ATO, FTO etc.), doped indium oxide (as ITO), doping weisspiessglanz, doping zinc-oxide, titanium dioxide.
Such multi-factor structure complex conductive fillers can utilize absorbing material to improve its capability of electromagnetic shielding to electromagnetic absorptive character and electro-conductive material further to electromagnetic reflecting properties, it has, and quality is light, cost is low, advantage such as shielding bandwidth, advantages of good shielding performance etc., has very large using value in electromagnetic shielding composite material field.
Embodiment
By specific examples, the invention will be further described.
Embodiment 1:
Adopt coprecipitation method at hollow glass micropearl coating surface one deck Z 250, adopt electroless plating at its coating surface one deck silver again, preparation multi-factor structure composite conductor filler-hollow glass micropearl/Z 250/silver, wherein the mass percent of hollow glass micropearl, Z 250 and silver is respectively 35%, 35% and 30%, by respective quality ratio ratio calculation, weigh each raw material.Be the ratio mixing of 3: 2 in amount of substance ratio by the iron nitrate of same concentrations, solution of ferrous chloride, add wash, the hollow glass micropearl of roughening treatment, drip precipitation agent NaOH solution, reaction 15min, then filter, wash, dry, obtain hollow glass micropearl/Z 250 composite granule.Configuration concentration is the silver ammino solution of 0.05mol/L, adds hollow glass micropearl/Z 250 composite granule, stirs, is heated to 45 DEG C, drip reductive agent formaldehyde, reaction 15min, then filters, washs, dry, obtains hollow glass micropearl/Z 250/argentum composite powder body.
Embodiment 2:
Adopt hydrothermal method at carbon fiber surface plating one deck Z 250, adopt electroless plating at its coating surface one deck silver again, preparation multi-factor structure composite conductor filler-carbon fiber/Z 250/silver, wherein the mass percent of carbon fiber, Z 250 and silver is respectively 40%, 35% and 25%, by respective quality ratio ratio calculation, weigh each raw material.Be the ratio mixing of 5: 3 in amount of substance ratio by the iron nitrate of same concentrations, solution of ferrous chloride; add urea and stir and obtain clear solution; then solution is placed in autoclave; add carbon fiber; and add suitable quantity of water; compactedness is made to be 0.65; sealed reactor; pass into nitrogen (as protection gas), high-speed stirring, is heated to 140 DEG C by solution in reactor; maintain atmospheric pressure at 6 ~ 7 normal atmosphere; reaction 2h, then filters, washs, dry, obtains carbon fiber/Z 250 composite granule.Configuration concentration is the silver ammino solution of 0.05mol/L, adds carbon fiber/Z 250 composite granule, stirs, is heated to 60 DEG C, drips reductive agent formaldehyde, reaction 10min, then filters, washs, dry, obtains carbon fiber/Z 250/argentum composite powder body.
Embodiment 3:
Adopt sol-gel method at fiberglass surfacing plating one deck barium ferrite (BaFe
12o
19), adopt electroless plating at its coating surface one deck silver again, preparation multi-factor structure composite conductor filler-glass fibre/barium ferrite/silver, wherein the mass percent of glass fibre, barium ferrite and silver is respectively 40%, 40% and 20%, by respective quality ratio ratio calculation, weigh each raw material.Nitrate of baryta, iron nitrate and the citric acid ratio according to mol ratio 1: 12: 13 is mixed, add distilled water and stir 20min, make it to dissolve completely, dripping ammoniacal liquor adjust ph is 7, make solution become vitreosol, and at 75 DEG C constant temperature water bath 2h, then by cleaning, roughening treatment glass fibre be placed in sol solution, under stirring, make Sol-gel Coated in fiberglass surfacing; Then be placed in baking oven, at 120 DEG C of dry 20h, obtain chocolate xerogel; Crucible put into by xerogel, through 450 DEG C of thermal pretreatment 1h in retort furnace, then carries out sintering processes 2h at 850 DEG C, takes out sample and grinds, obtain glass fibre/barium ferrite composite granule after cooling.Configuration concentration is the silver ammino solution of 0.03mol/L, adds glass fibre/barium ferrite composite granule, stirs, is heated to 60 DEG C, drips reductive agent formaldehyde, reaction 10min, then filters, washs, dry, obtains glass fibre/barium ferrite/argentum composite powder body.
Embodiment 4:
Adopt sol-gel method in mica surface plating one deck barium ferrite, adopt the stannic oxide (ATO) that heterogeneous nucleation process adulterates at its coating surface one deck weisspiessglanz again, preparation multi-factor structure composite conductor filler-mica/barium ferrite/ATO, wherein the mass percent of mica, barium ferrite and ATO is respectively 30%, 50% and 20%, by respective quality ratio ratio calculation, weigh each raw material.The preparation of mica/barium ferrite composite granule is see embodiment 3.Join in distilled water by mica/barium ferrite powder, dispersed with stirring forms suspension liquid, heats 60 DEG C; By SnCl
45H
2o and SbCl
3it is in the hydrochloric acid soln of 20% that the ratio being 5: 1 in amount of substance ratio is dissolved in concentration, forms transparent strongly acidic solution, and is added dropwise in the suspension liquid of mica/barium ferrite powder; Drip sodium hydroxide solution again, maintaining pH value is 4, and Keep agitation reaction 30min; By solution at the still aging 12h of room temperature, then filter, gained filter cake priority distilled water and ethanol wash are for several times; Gained filter cake dry 10h at 80 DEG C after washing, obtains dry powder; Finally by dry powder thermal treatment 30min at 800 DEG C, obtain mica/barium ferrite/ATO composite granule.
Claims (5)
1. multi-factor structure complex conductive fillers one inorganic powder kernel/magneticsubstance coating/electro-conductive material coating.The magneticsubstance of ripple is inhaled at inorganic powder surface plating one deck, then plating layer of conductive material.
2. a multi-factor structure complex conductive fillers, it is characterized in that: such complex conductive fillers can utilize absorbing material to improve its capability of electromagnetic shielding to electromagnetic absorptive character and electro-conductive material further to electromagnetic reflecting properties, have that quality is light, cost is low, advantage such as shielding bandwidth, advantages of good shielding performance etc.
3. multi-factor structure complex conductive fillers according to claim 1, is characterized in that: inorganic powder is the inorganic materials of the light weights such as hollow glass micropearl, mica, carbon fiber, flake graphite, carbon nanotube, glass fibre.
4. multi-factor structure complex conductive fillers according to claim 1, is characterized in that: magneticsubstance is Ni, Fe, Co, Cr, Nd, Mo, Ni-P, Co-P, Ni-Co-P, Co-W-P, barium ferrite, Z 250, iron carbonyl etc.
5. a multi-factor structure complex conductive fillers according to claim 1, is characterized in that: the metals such as electro-conductive material is silver, nickel, copper or the inorganic oxide such as doped stannum oxide (as ATO, FTO etc.), doped indium oxide (as ITO), doping weisspiessglanz, doping zinc-oxide, titanium dioxide.
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| CN105776892A (en) * | 2016-01-29 | 2016-07-20 | 中北大学 | Magnetic Ag-plated glass bead and preparing method thereof |
| CN105848314A (en) * | 2016-06-07 | 2016-08-10 | 安邦电气股份有限公司 | Temperature self-limited heating cable capable of electric energy saving |
| CN106497019A (en) * | 2016-10-06 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of electromagnetic shielding material |
| CN106751935A (en) * | 2016-12-12 | 2017-05-31 | 铜仁学院 | A kind of composite microwave absorbing material and preparation method thereof |
| CN106752804A (en) * | 2017-01-25 | 2017-05-31 | 山东凯盛新材料股份有限公司 | High temperature resistant, antistatic PEKK powdery paints and preparation method thereof |
| CN106926545A (en) * | 2017-03-24 | 2017-07-07 | 上海源紊新能源科技有限公司 | A kind of improved suction antimagnetic sheet material of ripple |
| CN107051343A (en) * | 2016-12-06 | 2017-08-18 | 青岛大学 | The preparation method of the sour nickel@ferriferrous oxide composite materials of the carbon@cobalts of multi-layer core-shell structure |
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| CN109348696A (en) * | 2018-10-15 | 2019-02-15 | 安徽理工大学 | A kind of preparation method of Fe2O3 doping stannic oxide/nano combined absorbing material of redox graphene |
| CN110002458A (en) * | 2019-04-03 | 2019-07-12 | 中南大学 | A kind of porous microsphere/ferrite/conductive layer composite material for microwave absorption |
| CN110256102A (en) * | 2019-07-11 | 2019-09-20 | 郭建中 | A kind of preparation method of novel TiN base efficient and light weight absorbing material |
| CN110257007A (en) * | 2019-07-18 | 2019-09-20 | 韦玉伍 | A kind of barium ferrite of low-density-iron powder composite wave-suction material |
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| CN111004555A (en) * | 2019-12-26 | 2020-04-14 | 中国人民解放军军事科学院国防工程研究院工程防护研究所 | Radioactive pollution control and removal material and preparation method thereof |
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| CN115337878A (en) * | 2021-05-12 | 2022-11-15 | 中国科学院理化技术研究所 | Composite hollow microsphere with layered composite spherical shell structure and preparation method and application thereof |
| CN115340748A (en) * | 2021-05-12 | 2022-11-15 | 中国科学院理化技术研究所 | Light high-strength electromagnetic shielding composite material based on conductive hollow microspheres and preparation method and application thereof |
| CN115337878B (en) * | 2021-05-12 | 2024-02-20 | 中国科学院理化技术研究所 | Composite hollow microsphere with layered composite spherical shell structure and preparation method and application thereof |
| CN115340748B (en) * | 2021-05-12 | 2024-05-03 | 中国科学院理化技术研究所 | Light high-strength electromagnetic shielding composite material based on conductive hollow microspheres and preparation method and application thereof |
| CN114025600A (en) * | 2021-11-08 | 2022-02-08 | 南昌三瑞智能科技有限公司 | Electromagnetic shielding rotating part conductive lap joint module of power motor of unmanned aerial vehicle |
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| CN115213396B (en) * | 2022-08-16 | 2023-10-24 | 湖南湘投轻材科技股份有限公司 | Electromagnetic shielding material and preparation method thereof |
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Application publication date: 20160127 |