CN104194275A - Preparation method for high-resisting and high-attenuation-resisting backing material - Google Patents
Preparation method for high-resisting and high-attenuation-resisting backing material Download PDFInfo
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- CN104194275A CN104194275A CN201410464380.4A CN201410464380A CN104194275A CN 104194275 A CN104194275 A CN 104194275A CN 201410464380 A CN201410464380 A CN 201410464380A CN 104194275 A CN104194275 A CN 104194275A
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Abstract
The invention discloses a preparation method for a high-resisting and high-attenuation-resisting backing material and belongs to the technical field of materials. According to the preparation method disclosed by the invention, by using a CVD (Chemical Vapor Deposition) method and taking ethanol as a carbon source, three-dimensional graphene with large size and a porous multistage structure is grown by exploring the growth temperature, the growth time, the flow of oxygen gas, the annealing speed and other factors and taking foamed nickel as a catalyst and a temperature carrier; a graphene framework is filled with a tungsten powder and epoxy resin compound; the sound absorption property of the a tungsten powder and epoxy resin compound as a traditional backing material is improved by using the porous multistage structure and good electric mass transfer performance of the three-dimensional graphene, and further the high-resisting and high-attenuation-resisting backing material according with actual application of an energy transducer is prepared. Due to the introduction of a graphene three-dimensional continuous framework, the material has better electrical conductivity and larger conjugate field; electronics can freely move in the period; sound energy can be converted into electric energy which is finally converted into heat for dissipating, so the material is excellent in sound absorption effect.
Description
Technical field
The invention belongs to material technology field, relate to a kind of novel method of preparing the high attenuating material of high resistance.
Background technology
Graphene (graphene) is individual layer two dimension (2D) carbonaceous material by the tightly packed one-tenth of carbon atom.Owing to having the performances such as fabulous electricity, optics, machinery, Graphene is extensively concerned.Integrate 2D Graphene and build the Graphene assembly with specific three dimensional (3D) structure, and then the functional device of processability excellence is significant for the macroscopic view application of expanding Graphene.3D structure can be given the character of Graphene assembly uniqueness, as snappiness, porousness, high reactivity specific surface area, excellent mass-transfer performance etc.
Research at present shows; 3D Graphene and matrix material thereof possess the intrinsic character of Graphene, have the performance more superior compared with 2D grapheme material and more wide application prospect at energy storage, catalyzed reaction, environment protection and flexibility/aspects such as scalable electro-conductive material.
Carbon material has been widened the research direction of carbon material in the Application Areas of sound-absorbing material, there are some researches show, carbon material such as carbon nanotube injects with minute quantity the sound absorption damping that traditional architecture sound-absorbing material polyurethane foam can strongthener, improves Young's modulus and the pressure-strain of material; Ratio mixed grinding by the graphene oxide after sodium borohydride reduction and polyaniline in 2: 4, evenly be coated on cloth or film, bake drying at 60 DEG C, obtain graphene/polyaniline sound-absorbing material between 125-4000 Hz maximum sound absorption coefficient up to 80%, and material conductivity is better, and sound absorbing capabilities is higher.
Summary of the invention
The object of this invention is to provide the preparation method of the high decay of a kind of high resistance back lining materials.The method is utilized CVD method, using ethanol as carbon source, by probing into growth temperature, growth time, carrier gas Ar, H
2the factor such as flow and annealing speed, taking nickel foam as catalyzer and template carrier, grow large size, there is the three-dimensional grapheme of poroid multilevel hierarchy.In Graphene skeleton, fill tungsten powder and epoxy resin composite, utilize the multistage cavernous structure of three-dimensional grapheme and good electricity mass-transfer performance, improve the sound absorbing capabilities of traditional back lining materials tungsten powder and epoxy resin composite, prepare the back lining materials of the high decay of high resistance that meets transverter practical application.
The object of the invention is to be achieved through the following technical solutions:
Technical scheme one: the preparation of three-dimensional grapheme/tungsten powder/epoxy resin composite (G-Epoxy/ W/Epoxy) film, its key step is as follows:
One, with CVD method growing three-dimensional Graphene (Ni-G skeleton):
(1) cut 10 cm × 10 cm nickel foam, acetone ultrasonic cleaning 10 ~ 20 min tri-times, dries stand-by.Adopt ethanol as carbon source, with Ar, H
2as carrier gas, nickel foam is as catalyzer and carrier, is 100 ~ 200 sccm, H at 900 ~ 1100 DEG C, Ar flow velocity
2flow velocity is to nickel foam annealing 10 ~ 30min, to eliminate the nickel foam oxidized part in surface and unrelieved stress under 100 ~ 200 sccm.
(2) be 50 ~ 200 sccm, H at 700 ~ 900 DEG C, Ar flow velocity
2flow velocity is under 0 ~ 150 sccm, and ethanol is sent in boiler tube in bubbling mode, keeps growth 5 ~ 30 min.
(3) close ethanol valve, stop the supply of ethanol carbon source, with the speed cooling of 5 ~ 30 DEG C/min, obtain controlled big scale, the Graphene skeleton of the number of plies going out taking nickel foam skeleton as template growth.
Two, the preparation of three-dimensional grapheme foam framework (GF-Epoxy skeleton):
(1) preparation is containing the ethanolic soln of 1 ~ 10wt.% Epoxy, the Graphene that contains Ni skeleton that CVD is grown is immersed wetting, take out in 30 ~ 50 DEG C of baking ovens and dry 10 ~ 30 min, wetting, drying operation 3 ~ 5 times repeatedly, on Graphene surface, parcel one deck Epoxy supports as skeleton, forms Ni-G-Epoxy mixture.
(2) at 60 ~ 90 DEG C, process Ni-G-Epoxy mixture 3 ~ 10 h with 3mol/L HCl, etching N i, formation has the skeleton structure of the GF-Epoxy of certain flintiness.
The preparation of three, three-dimensional grapheme/epoxy resin/tungsten powder mixture (GF-Epoxy/W/Epoxy) film:
(1) choose the tungsten powder of particle diameter 5 ~ 50 μ m, be mixed with tungsten powder and epoxy resin composition that tungsten powder mass concentration is 60 ~ 95 wt.%, stir, vacuumize 3 ~ 10min and remove bubble.
(2) the bulk Graphene foam framework of preparing is cut into 1 cm × 1cm ~ 3cm × 3cm fritter, be placed in mould, pour tungsten powder and epoxy resin composition into, guarantee the tungsten powder energy submergence Graphene skeleton under precipitation, wait solidifying after 30 ~ 120 min, epoxy-resin systems is difficult for flowing, with pressing machine by film compacting, continue to solidify 2 ~ 6 h, make in the multistage three-dimensional grapheme skeleton of embedding that tungsten powder and epoxy systems are firm.
(3) film is taken out from mould, with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, making film thickness is 0.5 ~ 2 mm, poor the remaining between 0.2 ~ 1mm of all film thicknesses of preparing.
Technical scheme two: contain the preparation of three-dimensional grapheme/tungsten powder/epoxy resin composite (Ni-G/W/Epoxy) film of Ni skeleton, its key step is as follows:
One, with CVD method growing three-dimensional Graphene (Ni-G skeleton):
(1) cut 10 cm × 10 cm nickel foam, acetone ultrasonic cleaning 10 ~ 20 min tri-times, dries stand-by.Adopt ethanol as carbon source, with Ar, H
2as carrier gas, nickel foam is as catalyzer and carrier, is 100 ~ 200 sccm, H at 900 ~ 1100 DEG C, Ar flow velocity
2flow velocity is to nickel foam annealing 10 ~ 30min, to eliminate the nickel foam oxidized part in surface and unrelieved stress under 100 ~ 200 sccm.
(2) be 50 ~ 200 sccm, H at 700 ~ 900 DEG C, Ar flow velocity
2flow velocity is under 0 ~ 150 sccm, and ethanol is sent in boiler tube in bubbling mode, keeps growth 5 ~ 30 min.
(3) close ethanol valve, stop the supply of ethanol carbon source, with the speed cooling of 5 ~ 30 DEG C/min, obtain controlled big scale, the Graphene skeleton of the number of plies going out taking nickel foam skeleton as template growth.
Two, contain the preparation of three-dimensional grapheme // tungsten powder/epoxy resin (Ni-G/W/Epoxy) complex thin film of Ni skeleton:
(1) choose the tungsten powder of particle diameter 5 ~ 50 μ m, be mixed with tungsten powder and epoxy resin composition that tungsten powder concentration is 60 ~ 95 wt.%, stir, vacuumize 3 ~ 10min and remove bubble.
(2) Ni-G skeleton CVD being grown into cuts into 1 cm × 1cm ~ 3cm × 3cm fritter, be placed in mould, pour tungsten powder and epoxy resin composition into, guarantee the tungsten powder energy submergence Ni skeleton under precipitation, wait solidifying after 30 ~ 120 min, epoxy-resin systems is difficult for flowing, with pressing machine by film compacting, continue to solidify 2 ~ 6 h, the embedding that tungsten powder and epoxy systems are firm is contained in the three-dimensional grapheme of Ni skeleton.
(3) film is taken out from mould, with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, making film thickness is 0.5 ~ 2 mm, and the thickness difference of different films remains between 0.2 ~ 1mm.
In the present invention, described Epoxy is that 3:1 mixes by Epoxy A and Epoxy B according to mass ratio.
The three-dimensional grapheme that CVD method grows can provide big area crystal formation perfect graphene sheet layer, has the mass-transfer performance of snappiness, porousness, high reactivity specific surface area, excellence.The present invention introduces Graphene in traditional back lining materials tungsten powder and epoxy resin, utilize structural performance and the physical property of three-dimensional grapheme, increase the loss of sound wave in material, can improve the sound attenuation performance of traditional back lining materials tungsten powder and epoxy cpd, thereby prepare the back lining materials of the high decay of high resistance that meets transverter practical application.This material is not singly the damped motion sound absorption of simple dependence sound wave and material, utilizes after absorbed acoustic wave energy yet, relies on the resonant interaction of molecule and conductivity to consume the energy of sound wave.Due to the three-dimensional introducing of skeleton continuously of Graphene, this material has good specific conductivity and larger conjugated system, electronics can during free movement, acoustic energy can be converted into electric energy and finally be converted into dissipation of heat and fall, thereby this material has good acoustically effective.
Back lining materials in transverter mainly contains two purposes: one, mate with piezoelectric crystal material, reduce the vibration number of wafer, thereby improve the frequency span of probe; Two, the sound wave that absorption pressure electroceramics is launched dorsad, reduces the impact of clutter on probe dorsad, improves the reliability detecting.The present invention utilizes the auxiliary sound absorbing capabilities that improves back lining materials of Graphene, prepares the high attenuating material of high resistance, makes the transverter of preparing have advantages of that pulse is short, bandwidth.
The present invention has following advantage:
1, use CVD method, taking ethanol as carbon source, Ar and H
2for carrier gas, can prepare big scale, high quality, the controlled three-dimensional grapheme of the number of plies by regulating and controlling the factors such as growth temperature and growth time, carrier gas flux, annealing temperature, rate of temperature fall, preparation process high yield is controlled, for the preparation of back lining materials provides skeleton structure.
2, the sheet layer graphene of preparing has good pleated structure, and the poroid multilevel hierarchy providing contributes to the damping vibration of sound wave in material.
3,, because Graphene has good electricity mass-transfer performance, complex thin film of the present invention can utilize the resonant interaction of molecule and conductivity to increase the waste of energy of sound wave.Because this thin-film material has good specific conductivity and larger conjugated system, electronics can during free movement, acoustic energy is converted into electric energy and is finally converted into dissipation of heat and falls, thereby realize the superior sound absorbing capabilities of this material.
4, by particle diameter and the content of W in regulation and control GF-Epoxy/W/Epoxy complex thin film and Ni-G/W/Epoxy complex thin film, can locate the thin-film material of preparing different impedances and pad value, thereby mate different piezoquartzs, prepare the ultrasonic transducer of different performance.
5,, due to the introducing of Graphene skeleton and preparation method's improvement, the high resistance of 11.8 ± 0.1 MRayl under 10MHz frequency, the height decay back lining materials of 38.86 ± 1.88 dB/cm*MHz have been prepared.
Brief description of the drawings
Fig. 1 is the preparation process schematic diagram that does not contain the GF-Epoxy/W/Epoxy complex thin film of Ni skeleton;
Fig. 2 is the photo of Ni foam;
Fig. 3 is the Ni-G photo after CVD growth;
Fig. 4 is the photo that forms Ni-G-Epoxy skeleton at Ni – G surface-coated one deck Epoxy;
Ni in Ni-G-Epoxy is etched away the photo that forms GF-Epoxy skeleton by Fig. 5;
Fig. 6 is the Raman spectrum of Graphene on Ni-G skeleton;
Fig. 7 is low power and the high power SEM figure of Graphene on Ni-G skeleton;
Fig. 8 is the variation with Tungsten Powder Size containing the specific acoustic resistance of three-dimensional grapheme/tungsten powder/epoxy resin composite film of Ni skeleton;
Fig. 9 is the variation with Tungsten Powder Size containing the sound attenuation of three-dimensional grapheme/tungsten powder/epoxy resin composite film of Ni skeleton;
Figure 10 is the not variation with Tungsten Powder Size containing the specific acoustic resistance of three-dimensional grapheme/tungsten powder/epoxy resin composite film of Ni skeleton;
Figure 11 is the not variation with Tungsten Powder Size containing the sound attenuation of three-dimensional grapheme/tungsten powder/epoxy resin composite film of Ni skeleton;
Figure 12 is the not variation with tungsten powder content containing the specific acoustic resistance of three-dimensional grapheme/20 μ m tungsten powder/epoxy resin composite film of Ni skeleton;
Figure 13 is the not variation with tungsten powder content containing the sound attenuation of three-dimensional grapheme/20 μ m tungsten powder/epoxy resin composite film of Ni skeleton.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described; but be not limited to this; every technical solution of the present invention is modified or is equal to replacement, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
embodiment 1:
The present embodiment provides a kind of preparation method who does not contain the GF-Epoxy/W/Epoxy complex thin film of Ni skeleton, and as shown in Figure 1, concrete steps are as follows:
One, CVD method growing three-dimensional Graphene (Ni-G skeleton):
Cut 10 cm × 10 cm nickel foam, acetone ultrasonic cleaning 10 min tri-times, dries stand-by.Nickel foam is rolled into spirrillum and pushes in the middle of stove, eliminate the nickel foam oxidized part in surface and unrelieved stress for activation nickel foam, it is 100sccm, H that Ar flow velocity is set
2flow velocity is 100 sccm, at 1000 DEG C to nickel foam annealing 20min.Stove is cooled to 875 DEG C with 10min, open ethanol valve, regulating Ar flow velocity is 180sccm, H
2flow velocity is 20 sccm, keeps growth 25min.After growth, close ethanol valve, with the rate of temperature fall of 15 DEG C/min, Graphene is separated out, the Graphene number of plies of preparing is between 5-10 layer.
Two, the preparation of three-dimensional grapheme foam (GF-Epoxy) skeleton:
Get 3.75g Epoxy A glue in watch-glass, add 95g ethanol agitation and dilution 10min, add 1.25g Epoxy B glue to continue agitation and dilution 10min, the Graphene containing Ni skeleton that CVD is grown is immersed in alcohol dilution liquid, take out in 45 DEG C of baking ovens and dry 10min, repeatable operation 3 times, forms Ni-G-Epoxy mixture.Preparation 3mol/L HCl, the Ni at 90 DEG C in etching N i-G-Epoxy washes away the remaining HCl in GF-Epoxy surface with clear water after Ni etching is complete, in the baking oven of 45 DEG C, dries.
Three, do not contain the preparation of three-dimensional grapheme/12 μ m tungsten powder/epoxy resin composites (GF-Epoxy/W/Epoxy) film of Ni skeleton:
Get the tungsten powder of 10g particle diameter 12 μ m, add 1.875 g Epoxy A glue and 0.625 g Epoxy B glue, stir, be mixed with tungsten powder and the epoxy resin composition of 80 wt.%, vacuumize 5 min and remove bubble.The bulk GF-Epoxy skeleton of preparing is cut into 3cm × 3cm fritter, be placed in mould, pour the mixture of the 80 wt.% W/Epoxy that are mixed into into, guarantee the tungsten powder energy submergence Graphene skeleton under precipitation, wait solidifying after 30min, epoxy-resin systems is difficult for flowing, with pressing machine by thin film system compacting, continue to solidify 4h, make in the multistage three-dimensional grapheme skeleton of embedding that tungsten powder and epoxy systems are firm.Film is taken out from mould, and with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, making film thickness is 1 mm.
Ni foam presents metalluster, provides the Growh framework of Graphene, as shown in Figure 2.Through CVD method, at nickel foam skeleton surface coverage graphene sheet layer, the number of plies can be regulated by factors such as carrier gas flux, growth temperature and time, annealing rates in process of growth.Fig. 3 is the picture of the Ni-G after growth, black, present the color of carbon material, visible Graphene uniform fold in Ni foam surface, determine through Raman spectrum, as Fig. 6, according to the characteristic peak G of Graphene, 2D peak, the Graphene growing has very regular structure, and can estimate from the peak height ratios at G and 2D peak the Graphene number of plies of preparing is 5-10 layer.Scanning electron microscope diagram sheet by Fig. 7 is observed the epontic Graphene of Ni skeleton, and visible Graphene has good laminated structure and very high quality.
Because Graphene skeleton matter is soft, be the skeleton structure that ensures that in subsequent disposal it is intact, wrap up in one deck thin layer Epoxy(Fig. 4 at Ni-G Skeleton Table bread in advance), then use HCl etching N i skeleton, form GF-Epoxy skeleton (Fig. 5).
embodiment 2:
The present embodiment provides a kind of preparation method of three-dimensional grapheme/tungsten powder/epoxy resin composite (Ni-G/W/Epoxy) film containing Ni skeleton, and concrete steps are as follows:
One, CVD method growing three-dimensional Graphene (Ni-G skeleton):
Cut 10 cm × 10 cm nickel foam, acetone ultrasonic cleaning 10 min tri-times, dries stand-by.Nickel foam is rolled into spirrillum and pushes in the middle of stove, eliminate the nickel foam oxidized part in surface and unrelieved stress for activation nickel foam, it is 100sccm, H that Ar flow velocity is set
2flow velocity is 100 sccm, at 1000 DEG C to nickel foam annealing 20min.Stove is cooled to 875 DEG C with 10min, open ethanol valve, regulating Ar flow velocity is 180sccm, H
2flow velocity is 20 sccm, keeps growth 25min.After growth, close ethanol valve, with the rate of temperature fall of 15 DEG C/min, Graphene is separated out, the Graphene number of plies of preparing is at 5-10 interlayer.
two,contain the preparation of three-dimensional grapheme/12 μ m tungsten powder/epoxy resin composites (Ni-G/W/Epoxy) film of Ni skeleton:
Get the tungsten powder of 10g particle diameter 12 μ m, add 1.875 g Epoxy A glue and 0.625 g Epoxy B glue, stir, be mixed with tungsten powder and the epoxy resin composition of 80 wt.%, vacuumize 5 min and remove bubble.The bulk Ni-G skeleton of preparing is cut into 3cm × 3cm fritter, be placed in mould, pour the mixture of the 80 wt.% W/Epoxy that are mixed into into, guarantee the tungsten powder energy submergence Graphene skeleton under precipitation, wait solidifying after 30min, epoxy-resin systems is difficult for flowing, with pressing machine by thin film system compacting, continue to solidify 4h, make in embedding Ni-G skeleton that tungsten powder and epoxy systems are firm.Film is taken out from mould, and with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, making film thickness is 1 mm.
Fig. 8-11 are respectively the multistage three-dimensional grapheme to contain Ni skeleton and are not filling matrix containing the multistage three-dimensional grapheme of Ni skeleton, the sound absorbing capabilities of the film that the tungsten powder of screening different-grain diameter is prepared into.The acoustically effective of two kinds of skeletons of contrast, selects the not Graphene skeleton containing Ni skeleton.According to the Tungsten Powder Size filtering out, be prepared into Graphene/tungsten powder/epoxy resin composite film of the different tungsten powder content of this particle diameter, test its acoustically effective, as shown in Figure 12-13.Prepare, insert in Graphene skeleton when the tungsten powder with 80 wt.% 20 μ m and epoxy resin composite, institute's made membrane is under 10MHz frequency, and specific acoustic resistance reaches 11.8 ± 0.1MRayl, and acoustic attenuation coefficient reaches 38.86 ± 1.88 dB/cm*MHz.
Claims (10)
1. a preparation method for the high decay of high resistance back lining materials, is characterized in that described preparation method's step is as follows:
One, with CVD method growing three-dimensional Graphene:
(1) adopt ethanol as carbon source, with Ar, H
2as carrier gas, nickel foam is as catalyzer and carrier, is 100 ~ 200 sccm, H at 900 ~ 1100 DEG C, Ar flow velocity
2flow velocity is to nickel foam annealing 10 ~ 30min under 100 ~ 200 sccm;
(2) be then 50 ~ 200 sccm, H at 700 ~ 900 DEG C, Ar flow velocity
2flow velocity is under 0 ~ 150 sccm, and ethanol is sent in boiler tube in bubbling mode, keeps growth 5 ~ 30 min;
(3) close ethanol valve, stop the supply of ethanol carbon source, with the speed cooling of 5 ~ 30 DEG C/min, obtain the Graphene skeleton going out taking nickel foam skeleton as template growth;
Two, the preparation of three-dimensional grapheme foam framework:
(1) preparation is containing the ethanolic soln of 1 ~ 10 wt.% Epoxy, the Graphene that contains Ni skeleton is immersed wetting, take out in 30 ~ 50 DEG C of baking ovens and dry 10 ~ 30 min, wetting, drying operation 3 ~ 5 times repeatedly, on Graphene surface, parcel one deck Epoxy supports as skeleton, forms Ni-G-Epoxy mixture;
(2) at 60 ~ 90 DEG C, process Ni-G-Epoxy mixture 3 ~ 10 h with HCl, etching N i, the skeleton structure of formation GF-Epoxy;
The preparation of three, three-dimensional grapheme/epoxy resin/tungsten powder complex thin film:
(1) preparation tungsten powder mass concentration is tungsten powder and the epoxy resin composition of 60 ~ 95 wt.%, stirs, and vacuumizes 3 ~ 10min and removes bubble;
(2) the grapheme foam skeleton of preparing is cut into fritter, be placed in mould, pour tungsten powder and epoxy resin composition into, guarantee the tungsten powder energy submergence Graphene skeleton under precipitation, after solidifying 30 ~ 120 min, by film compacting, continue to solidify 2 ~ 6 h;
(3) film is taken out from mould, with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, obtain Graphene/epoxy resin/tungsten powder complex thin film.
2. the preparation method of the high decay of high resistance according to claim 1 back lining materials, is characterized in that described nickel foam is of a size of 10 cm × 10 cm.
3. the preparation method of the high decay of high resistance according to claim 1 back lining materials, is characterized in that described Tungsten Powder Size is 5 ~ 50 μ m.
4. the preparation method of the high decay of high resistance according to claim 1 back lining materials, is characterized in that described tile size is 1cm × 1cm ~ 3cm × 3cm.
5. the preparation method of the high decay of high resistance according to claim 1 back lining materials, is characterized in that described Graphene/epoxy resin/tungsten powder complex thin film thickness is 0.5 ~ 2 mm.
6. a preparation method for the high decay of high resistance back lining materials, is characterized in that described preparation method's step is as follows:
One, with CVD method growing three-dimensional Graphene:
(1) adopt ethanol as carbon source, with Ar, H
2as carrier gas, nickel foam is as catalyzer and carrier, is 100 ~ 200 sccm, H at 900 ~ 1100 DEG C, Ar flow velocity
2flow velocity is to nickel foam annealing 10 ~ 30min under 100 ~ 200 sccm;
(2) be then 50 ~ 200 sccm, H at 700 ~ 900 DEG C, Ar flow velocity
2flow velocity is under 0 ~ 150 sccm, and ethanol is sent in boiler tube in bubbling mode, keeps growth 5 ~ 30 min;
(3) close ethanol valve, stop the supply of ethanol carbon source, with the speed cooling of 5 ~ 30 DEG C/min, obtain the Graphene skeleton going out taking nickel foam skeleton as template growth;
Two, contain the preparation of three-dimensional grapheme // tungsten powder/epoxy resin composite film of Ni skeleton:
(1) preparation tungsten powder concentration is tungsten powder and the epoxy resin composition of 60 ~ 95 wt.%, stirs, and vacuumizes 3 ~ 10min and removes bubble;
(2) Graphene skeleton is cut into fritter, be placed in mould, pour tungsten powder and epoxy resin composition into, guarantee the tungsten powder energy submergence Ni skeleton under precipitation, after solidifying 30 ~ 120 min, by film compacting, continue to solidify 2 ~ 6 h;
(3) film is taken out from mould, with the unnecessary epoxy resin in sand papering upper strata, until Graphene skeleton exposes, with the unnecessary tungsten powder of sand papering lower floor, obtain the three-dimensional grapheme // tungsten powder/epoxy resin composite film containing Ni skeleton.
7. the preparation method of the high decay of high resistance according to claim 6 back lining materials, is characterized in that described nickel foam is of a size of 10 cm × 10 cm.
8. the preparation method of the high decay of high resistance according to claim 6 back lining materials, is characterized in that described Tungsten Powder Size is 5 ~ 50 μ m.
9. the preparation method of the high decay of high resistance according to claim 6 back lining materials, is characterized in that described tile size is 1cm × 1cm ~ 3cm × 3cm.
10. the preparation method of the high decay of high resistance according to claim 6 back lining materials, is characterized in that described three-dimensional grapheme // tungsten powder/epoxy resin composite film thickness containing Ni skeleton is 0.5 ~ 2 mm.
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Cited By (4)
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| CN104827021A (en) * | 2015-04-09 | 2015-08-12 | 山东师范大学 | Method for preparing high-conductivity stretchable sponge graphene-based electrode material |
| CN109320246A (en) * | 2018-11-01 | 2019-02-12 | 三峡大学 | A kind of high-temperature oxidation resistant graphite ceramic composite material and preparation method |
| CN110031923A (en) * | 2019-04-19 | 2019-07-19 | 电子科技大学 | Stretchable two-sided ultra wide band Terahertz absorbing material of formula and preparation method thereof |
| US11059948B2 (en) * | 2019-05-24 | 2021-07-13 | The Florida International University Board Of Trustees | Shape memory-based self-healing polymer composite reinforced with graphene foam |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104827021A (en) * | 2015-04-09 | 2015-08-12 | 山东师范大学 | Method for preparing high-conductivity stretchable sponge graphene-based electrode material |
| CN109320246A (en) * | 2018-11-01 | 2019-02-12 | 三峡大学 | A kind of high-temperature oxidation resistant graphite ceramic composite material and preparation method |
| CN110031923A (en) * | 2019-04-19 | 2019-07-19 | 电子科技大学 | Stretchable two-sided ultra wide band Terahertz absorbing material of formula and preparation method thereof |
| US11059948B2 (en) * | 2019-05-24 | 2021-07-13 | The Florida International University Board Of Trustees | Shape memory-based self-healing polymer composite reinforced with graphene foam |
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