CN106757283A - Foam metal-graphene composite material and preparation method thereof - Google Patents
Foam metal-graphene composite material and preparation method thereof Download PDFInfo
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- CN106757283A CN106757283A CN201510827299.2A CN201510827299A CN106757283A CN 106757283 A CN106757283 A CN 106757283A CN 201510827299 A CN201510827299 A CN 201510827299A CN 106757283 A CN106757283 A CN 106757283A
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Abstract
The invention discloses a kind of foam metal graphene composite material and preparation method thereof, the composite includes the Graphene film layer on foam metal basalis and substrate, and the foam metal graphene composite material is prepared with electrophoresis method.Specifically include defoam metal substrate surface greasy dirt and oxide, oxidation-reduction method prepare Graphene, modified graphene, in foam metal surface electrophoretic deposition Graphene.In certain electromagnetic wave band, on the one hand foam metal graphene composite material has the light porous of foam metal, a structural advantage that specific surface area is big and conductive performance is good, and the on the other hand compatible excellent electric conductivity of self-control Graphene, dielectric constant high and a large amount of defects and functional group's residual cause it to be more beneficial for the performances such as electromagnetic wave absorption.The composite has electromagnet shield effect higher, can be used as excellent electromagnetic shielding material.
Description
Technical field
The invention belongs to field of compound material, more particularly to a kind of Foam metal-graphene composite material and preparation method thereof.
Background technology
Porous foam metal is because with lighter weight, high specific surface area, preferable thermal conductivity and be subject to the extensive concern of researcher, it has the electric conductivity of metal, and multiple reflections and scattering loss are produced when the loose structure of three-dimensional communication causes electromagnetic wave incident in hole, there is the electromagnet shield effect suitable with solid metal plate in certain wave band.And the domestic research for porous foam metal for electromagnetic shielding material at present more lacks, it is necessary to carry out the functionalized application research of system to it.Since being found by Nobel Prize in physics winner Andre Geim and Kostya Novoselov from Graphene in 2004, its unique structure and excellent performance cause the extensive concern of researcher, and Graphene is with sp by carbon atom2Hydridization bonding form and by regular hexagon close-packed arrays into the individual layer two-dimension plane structure of honeycomb crystal lattice carbonaceous material, its excellent electrical conductivity, thermal conductivity, high-specific surface area and mechanical property cause that Graphene possesses huge application potential.Wherein due to the excellent electric conductivity of Graphene and dielectric constant high, and the distinctive defect of Graphene that chemically prepares and functional group's residual and the fermi level localization state that produces, this causes that Graphene has absorption and attenuation to electromagnetic wave.Therefore Graphene has as the application potential of electromagnetic shielding material.And it is less to be applied to electromagnetic shielding material research for Graphene at present.Especially in special application scenario, such as equipment needs to breathe freely when radiating, it is necessary to perforate radiating, in order to weaken the leakage of electromagnetic wave as far as possible, the shielding material of gas permeability there has been ample scope for abilities.
At present, the general fundamental type for being used as vent window design using wire netting or cellular cut-off waveguide window.Wire netting is used as two-dimentional conductive network, and its porosity is big, and suction ripple layer is short, and shield effectiveness is relatively low；And although the shield effectiveness of cellular cut-off waveguide window is preferably, its volume and weight is larger, it has not been convenient to installs and carries.The research of Graphene metallic composite is prepared to carbon graphite alkene and metal composite in recent years gradually to increase, its preparation method is using chemical vapor deposition（CVD) the direct growth Graphene in foam metal substrate, or make graphene solution is adhered on the metallic substrate by spraying method.Compared to composite of the invention, on its preparation method, compared to electrophoresis method, CVD method is expensive, instrumentation is complicated.
The content of the invention
It is an object of the invention to provide a kind of Foam metal-graphene composite material and preparation method thereof, the foam metal with lightweight, high-specific surface area, high conduction is combined preparation Foam metal-graphene composite material with the excellent Graphene of electric property.As shown in Figure 1, the loose structure of composite three dimensional connection produces multiple reflections and scattering loss when causing electromagnetic wave incident to material surface and inside, until being absorbed, the cooperative effect at the two interface causes that the composite has electromagnet shield effect higher in addition.
A kind of Foam metal-graphene composite material, it is characterised in that including the Graphene film layer in foam metal substrate and foam metal substrate, the composite is prepared by the method in foam metal basalis electrophoretic deposition Graphene.
A kind of preparation method of Foam metal-graphene composite material, it is characterised in that comprise the following steps：
(1) foam metal substrate is cleaned, oxide on surface is removed, it is standby that water cleans drying；
(2) modified graphene：By in Graphene and electrolyte addition organic solvent, ultrasonic 1 3h obtains electrophoresis liquid, and the concentration of Graphene is 0.1 ~ 0.6mg/ml in electrophoresis liquid, and the quality of electrolyte is 1 ~ 2 times of Graphene in electrophoresis liquid；
(3) electrophoretic deposition：With foam metal substrate as negative electrode, molybdenum electrode is anode, is placed in electrophoresis liquid, and the parallel distance of the interpolar of negative and positive two is 1 3cm, applies 200 ~ 350V of DC voltage, after 1 ~ 50min, takes out cathode material, is dried, and obtains Foam metal-graphene composite material.
The metal of described foam metal be copper, nickel, silver, iron, copper alloy, nickel alloy or aluminium alloy in one or more, and on foam metal per inch hole count be 20 ~ 110.
Electrolyte be cationic strong electrolyte, selected from calcium nitrate, magnesium nitrate, aluminum nitrate, dimethyl diallyl ammonium chloride and polydiallyldimethyl ammonium chloride one or more.
Described organic solvent is selected from one or two the mixing in methyl alcohol and isopropanol.
Beneficial effects of the present invention：
(1) it is substrate that the present invention uses lightweight, high-specific surface area, the foam metal of high conduction, wave mode Graphene is inhaled in the one layer of self-control of its surface electrophoretic deposition, make full use of the absorption and attenuation of the three-dimensional communication skeleton structure and graphene-structured dimensional effect of foam metal to electromagnetic wave, so that this kind of composite both combines the light porous of foam metal, the structural advantage that specific surface area is big and conductive performance is good, possess Graphene again as the excellent dimensional characteristic of carbon-based material, for the design of electromagnetic shielding material provides referential thinking.
(2) there is multiple reflections and scattering loss when porous three-dimensional connectivity structure causes electromagnetic wave incident in the composite, it is difficult to be escaped from material, until being absorbed, and because the addition of Graphene film layer increased an impedance mismatch interface, foam metal causes that the absorption loss of material is greatly increased with the synergy of both Graphenes, the shield effectiveness higher so as to impart the composite.
(3) Graphene is prepared from for improved Hummers methods, and the Graphene prepares that lamella is thinner compared with Hummers methods, and most thin to reach individual layer, thin Graphene has preferably inhales ripple efficiency.
(4) present invention can provide a kind of simple to operate, cycle is short, Foam metal-graphene composite material preparation technology with low cost, and intended application direction is electromagnetic shielding field.
(5) present invention uses electrophoretic deposition technique, and the method is simple to operate, cycle is short, with low cost, effect are obvious.
Brief description of the drawings
Fig. 1 is nickel foam pattern electromicroscopic photograph in embodiment 1.
Specific embodiment
Electromagnetic shielding test：Prepared composite is cut into 22.9mm*10.0mm, the test of electromagnet shield effect is carried out using vector network analyzer in 8 ~ 12GHz frequency ranges.
Technical scheme is further described below by way of specific embodiment：
Embodiment 1：
(1) foam nickel base is cleaned：PPI is 20,90,110, and thickness is three kinds of nickel foams of 1.5mm, and to be dipped in acetone and ethanol volume ratio be 1:30min is soaked to remove oxide on surface in the HCl solution of 6mol/L after ultrasonic cleaning 30min in 1 mixed solution, and it is standby that last deionized water cleans drying；
(2) Graphene is prepared：Using improved hummer ' s methods, the concentrated sulfuric acid of 50ml 98% is added in 250ml beakers, oil bath heating is added thereto to 10g K to 90 DEG C2S2O8With 10g P2O5, be cooled to 80 DEG C after dissolving, add 12g graphite powders reaction 4-5h, after be cooled to room temperature, add 2L deionized waters overnight, suction filtration, air drying, the graphite powder for being pre-oxidized.The graphite powder that 6g is pre-oxidized is added in the beaker for filling the 230ml concentrated sulfuric acids, after ice bath stirring 30min, 30g KMnO is gradually added4 Powder, is warming up to 40 DEG C, and stirring reaction 4h is placed in ice bath afterwards, adds the H of 1.0L deionized waters and 50ml 30%2O2, ice bath stir 1 ~ 2h, filtering, be washed till neutrality with the HCl and deionized water of the mol/L of 2L 1.Dialysis 3 days, air drying obtains graphene oxide（GO).
(3) 100mg GO are weighed to be put into 50ml deionized waters, ultrasonic 4h it is completely dispersed, adds the hydrazine hydrate of 91.6 mL 85%, stirring reaction 5h in 95 DEG C of oil baths, suction filtration, washing is fully dried at room temperature, obtains Graphene sample；
（4）Modified graphene：Weigh the Graphene and 45mg Mg (NO in 45mg steps 23)2*6H2O electrolyte is added in isopropanol, and the concentration for preparing Graphene is the electrophoresis liquid of 0.3mg/ml, and ultrasound 3h, obtains electrophoresis liquid at room temperature；
（5）Electrophoretic deposition：The above-mentioned nickel foam for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode nickel foam size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 2cm, applies DC voltage 300V, after 30min, cathode material is taken out, is spontaneously dried at room temperature, obtain nickel foam-graphene composite material；
Graphene film thickness is 0.5nm, and composite material surface pattern is shown in Fig. 1, it is seen that graphene layer is tightly combined with base metal nickel, and more uniform.
Sample electromagnet shield effect is tested with vector network analyzer, test frequency scope is 8 ~ 12GHz, and test result shows thickness for 1.5mm, and hole density is respectively 20PPI, electromagnet shield effect of the nickel foam-graphene composite material of 90PPI, 110PPI in 8 ~ 12GHz.In the range of 8 ~ 12GHz, the average SE of the 20PPI composites is about 13dB, and the average SE of the 90PPI composites is about 30dB, and the average SE of the 110PPI composites reaches as high as 42dB up to 35dB.
Embodiment 2：
Selection aperture is 110PPI, and thickness is respectively 0.5mm, and the nickel foam of 1.0mm, 1.5mm is research object, prepares nickel foam-graphene composite material, and specific experiment step is as follows：
（1）Cleaning foam nickel base：PPI is 110, and thickness is respectively 0.5mm, and it is 1 that three kinds of nickel foams of 1.0mm, 1.5mm are dipped in acetone with ethanol volume ratio:It is cleaned by ultrasonic 30min in 1 mixed solution, soaks 30min in the HCl solution of 6mol/L afterwards to remove oxide on surface, it is standby that last deionized water cleans drying；
（2）Graphene is prepared with embodiment 1;
（3）Modified graphene：Weigh the Graphene and 45mg Mg (NO in 45mg steps 23)2*6H2O electrolyte is added in isopropanol, and the concentration for preparing Graphene is the electrophoresis liquid of 0.3mg/ml, and ultrasound 3h, obtains electrophoresis liquid at room temperature；
（4）Electrophoretic deposition：The above-mentioned nickel foam for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode nickel foam size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 2cm, applies DC voltage 300V, after 30min, cathode material is taken out, is spontaneously dried at room temperature, obtain nickel foam-graphene composite material.
Embodiment 3：
Change nickel foam into PPI20, thickness is 1.5mm, and experimental procedure is specific as follows：
（1）Cleaning foam nickel base：PPI is 20, and thickness is respectively the nickel foam of 1.5mm, and to be dipped in acetone and ethanol volume ratio be 1:It is cleaned by ultrasonic 30min in 1 mixed solution, soaks 30min in the HCl solution of 6mol/L afterwards to remove oxide on surface, it is standby that last deionized water cleans drying；
（2）Graphene is prepared with embodiment 1;
（3）Modified graphene：Weigh the Graphene and 30mg Mg (NO in 15mg steps 23)2*6H2O electrolyte is added in isopropanol, and the concentration for preparing Graphene is the electrophoresis liquid of 0.1mg/ml, and ultrasound 3h, obtains electrophoresis liquid at room temperature；
（4）Electrophoretic deposition：The above-mentioned nickel foam for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode nickel foam size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 2cm, applies DC voltage 300V, after 30min, cathode material is taken out, is spontaneously dried at room temperature, obtain nickel foam-graphene composite material.
Graphene film thickness is 0.5nm, and electromagnet shield effect is Epileptic 18dB, and larger by pore size influences compared with the electromagnet shield effect for finding foamed composite compared with Example 1, under equal conditions, the smaller shield effectiveness in composite aperture is higher.
It is 20 to select two groups of specification PPI of nickel foam, and thickness is 1.5mm, and the concentration of Graphene changes 0.1mg/ml and 0.6mg/ml, voltage 300V, electrophoresis time 30min into respectively in electrolyte, and experimental procedure is ibid.Electromagnet shield effect is 8 ~ 14 dB and 13 ~ 23dB, the electromagnet shield effect of foamed composite is influenceed the Graphene thicknesses of layers difference of correspondence and deposition by electrophoresis concentration, also illustrate that electrophoresis process is wider to Graphene concentration requirement scope in electrolyte, is easy to practical operation.
Embodiment 4：
(1) foam copper substrate is cleaned：PPI is 110, thickness 1.5mm foam coppers are dipped in acetone and ethanol volume ratio is 1:It is cleaned by ultrasonic 30min in 1 mixed solution, soaks 30min in the HCl solution of 6mol/L afterwards to remove oxide on surface, it is standby that last deionized water cleans drying.
(2) Graphene is prepared：In 90 °C 98% of the concentrated sulfuric acid, add after being dissolved with 2 〇 8 and P2O5, under 80 °C, add crystalline flake graphite reaction 5h, suction filtration, washing, dry, obtain pre-oxidation graphite, pre-oxidation Graphene, 98% concentrated sulfuric acid and KMn 〇 4 are reacted into 1h under 10C, 4h is reacted under 20 °C, 0 and H2O2 of ratio is added, 2h is stirred under ice bath, filtering, washing is dialysed 2 days, dry, obtain graphene oxide；Graphene is reduced to obtain by sodium borohydride 95C stirring reactions are added in graphene oxide；
（3）Modified graphene：Weigh the Graphene and 45mg Mg (NO in 45mg steps 23)2*6H2O electrolyte is added in isopropanol, and the concentration for preparing Graphene is the electrophoresis liquid of 0.3mg/ml, and ultrasound 3h, obtains electrophoresis liquid at room temperature；
（4）Electrophoretic deposition：The above-mentioned foam copper for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode foam copper size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 2cm, apply DC voltage 250V, after 30min, cathode material is taken out, spontaneously dried at room temperature, obtain foam copper-graphene composite material, measure graphene film thickness be 1.2nm.
Sample electromagnet shield effect is tested with vector network analyzer, test frequency scope is 8 ~ 12GHz, electromagnet shield effect is：28 ~ 41dB, the electromagnet shield effect compared with the composite of embodiment 1 decreases.
Embodiment 5：
(1) cleaning foam iron base bottom：PPI is 10, thickness 1.5mm foamed irons are dipped in acetone and ethanol volume ratio is 1:It is cleaned by ultrasonic 10min in 3 mixed solution, soaks 10min in the HCl solution of 2mol/L afterwards to remove oxide on surface, it is standby that last deionized water cleans drying.
(2) Graphene is prepared with embodiment 1；
(3) modified graphene：Weigh in Graphene and 90mg Ca (NO3) 2*4H2O electrolyte the addition isopropanol in 90mg steps 2, the concentration for preparing Graphene is the electrophoresis liquid of 0.6mg/ml, and ultrasound 1h, obtains electrophoresis liquid at room temperature；
(4) electrophoretic deposition：The above-mentioned foamed iron for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode foamed iron size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 1cm, apply DC voltage 200V, after 1min, cathode material is taken out, spontaneously dried at room temperature, obtain foamed iron-graphene composite material, measure graphene film thickness be 0.2nm.
Sample electromagnet shield effect is tested with vector network analyzer, test frequency scope is 8 ~ 12GHz, electromagnet shield effect is：3~12dB。
Embodiment 6：
(1) foam aluminium alloy substrate is cleaned：PI is 60, thickness 1.5mm foam aluminium alloys are dipped in acetone and ethanol volume ratio is 3:It is cleaned by ultrasonic 50min in 1 mixed solution, soaks 50min in the HCl solution of 10mol/L afterwards to remove oxide on surface, it is standby that last deionized water cleans drying.
(2) Graphene is prepared with embodiment 1;
(3) modified graphene：Weigh in Graphene and 180mg polydiallyldimethyl ammonium chlorides electrolyte the addition methyl alcohol in 90mg steps 2, the concentration for preparing Graphene is the electrophoresis liquid of 0.6mg/ml, and ultrasound 5h, obtains electrophoresis liquid at room temperature；
(4) electrophoretic deposition：The above-mentioned foam aluminium alloy for cleaning up makees negative electrode, molybdenum electrode is anode, it is put into the electrophoresis liquid of step 3, negative electrode nickel foam size 22.9mm*10.0mm, the parallel distance of the interpolar of negative and positive two is 3cm, apply DC voltage 350V, after 50min, cathode material is taken out, spontaneously dried at room temperature, obtain foam aluminium alloy-graphene composite material, measure carbon graphite alkene film thickness be 10nm.
Sample electromagnet shield effect is tested with vector network analyzer, test frequency scope is 8-12GHz, and electromagnet shield effect is 5-31dB.
Claims (7)
1. Foam metal-graphene composite material, it is characterised in that including the graphene film in foam metal substrate and foam metal substrate, the composite is prepared by the method in foam metal basalis electrophoretic deposition Graphene.
2. Foam metal-graphene composite material according to claim 1, it is characterised in that the metal of described foam metal substrate is one or more in copper, nickel, silver, iron, copper alloy, nickel alloy or aluminium alloy.
3. Foam metal-graphene composite material according to claim 1, it is characterised in that hole count is 20 ~ 110 on described foam metal per inch.
4. the preparation method of Foam metal-graphene composite material according to claim 1, it is characterised in that comprise the following steps：
(1) foam metal substrate is cleaned, oxide on surface is removed, it is standby that water cleans drying；
(2) modified graphene：By in Graphene and electrolyte addition organic solvent, 1 ~ 5h of ultrasound obtains electrophoresis liquid, and the concentration of Graphene is 0.1 0.6mg/ml in electrophoresis liquid, and the quality of electrolyte is 1 ~ 2 times of Graphene in electrophoresis liquid；
(3) electrophoretic deposition：With foam metal as negative electrode, platinum electrode is anode, is placed in electrophoresis liquid, and the parallel distance of the interpolar of negative and positive two is 1 ~ 3cm, applies 200 ~ 350V of DC voltage, after 1 ~ 50min, takes out cathode material, is dried, and obtains Foam metal-graphene composite material.
5. the preparation method of Foam metal-graphene composite material according to claim 4, it is characterised in that described electrolyte is cationic strong electrolyte.
6. the preparation method of Foam metal-graphene composite material according to claim 5, it is characterised in that described cationic strong electrolyte is selected from calcium nitrate, magnesium nitrate, aluminum nitrate, dimethyl diallyl ammonium chloride and polydiallyldimethyl ammonium chloride one or more.
7. the preparation method of Foam metal-graphene composite material according to claim 4, it is characterised in that described organic solvent is selected from one or two the mixing in methyl alcohol and isopropanol.
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| CN108525615A (en) * | 2018-03-12 | 2018-09-14 | 东北石油大学 | A kind of preparation and its application of the Ni-based nitrogen-doped graphene aeroge of three-dimensional foam |
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- 2015-11-25 CN CN201510827299.2A patent/CN106757283A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107564874A (en) * | 2017-08-21 | 2018-01-09 | 硕阳科技股份公司 | A kind of flexible heat sink film and preparation method thereof and composite and flexible radiating film |
| CN107564874B (en) * | 2017-08-21 | 2019-08-23 | 硕阳科技股份公司 | A kind of flexible heat sink film and preparation method thereof and composite and flexible radiate film |
| CN108525615A (en) * | 2018-03-12 | 2018-09-14 | 东北石油大学 | A kind of preparation and its application of the Ni-based nitrogen-doped graphene aeroge of three-dimensional foam |
| CN108774496A (en) * | 2018-07-17 | 2018-11-09 | 天津北方烯旺材料科技有限公司 | A kind of graphene modified metal base oleophilic drainage material preparation method |
| CN109706507A (en) * | 2019-01-16 | 2019-05-03 | 华南理工大学 | A kind of two-dimentional MXene film and preparation method thereof with vertical channel structure |
| CN110820031A (en) * | 2019-11-19 | 2020-02-21 | 有研工程技术研究院有限公司 | Preparation method of miniature getter |
| CN112723495A (en) * | 2021-01-19 | 2021-04-30 | 南京环保产业创新中心有限公司 | Graphene oxide-Cu-Co/foamed titanium substrate composite electrode, and preparation method and application thereof |
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