CN102321994A - The nanometer Preparation Method made of paper that contains Graphene - Google Patents
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Abstract
The present invention provides a kind of nanometer Preparation Method made of paper that contains Graphene.Step comprises: the natural flake graphite 30g that gets particle diameter≤45 μ m is a raw material, with the dense H of 30ml
2SO
4, 10g K
2S
2O
8, 10g P
2O
5Mix and be placed in the flask, be heated to 80 ℃ after, in flask, add the natural flake graphite of particle diameter≤45 μ m that 20g dried, be heated to 80 ℃ oxidation reactions take place down; Adopt the humers method that its oxidation is obtained graphite oxide; Pressing mass fraction mixed with carbon nano-fiber than 1: 2; The suspension pressurization obtains wetting film; Obtain dry, complete nanometer paper after the oven dry.Electric conductivity of the present invention has improved about three times than original common nanometer paper electric conductivity; The interpolation of Graphene can increase the proportion of goods damageds of nanometer paper material; And the maximum loss rate of pure carbon nanofiber nanometer paper is 94.1%; Wave absorbed crest value reaches 12dB, and the maximum loss rate of nanometer paper is 96.5% behind the interpolation Graphene, and wave absorbed crest value reaches 13dB.
Description
(1) technical field
The present invention relates to material science, is exactly a kind of nanometer Preparation Method made of paper that contains Graphene specifically.
(2) background technology
" Graphene " has another name called " mono-layer graphite sheet ", be meant one deck intensive, be wrapped in the carbon atom on the honeycomb crystal lattice, carbon atom arrangement becomes two-dimensional structure, and is similar with the monoatomic layer of graphite.The physics professor Geim of Univ Manchester UK etc. utilizes the gold system " scaffold " of nano-scale; At first produce suspension single-layer graphene film on it; The graphene film of finding suspension is not " a two-dimentional flat structure "; But have " single layer structure of wavy ", and ascribe the stability of Graphene single layer structure to it in " the microcosmic distortion on the nanoscale ".Graphene decomposes the fullerene can become zero dimension, curls to form the CNT of one dimension, and stack can form three-dimensional graphite, and its basic unit as " carbon " family gets in touch the most a kind of form existence with other each forms.
Grapheme material has very excellent each item performance.The theoretical specific area of Graphene is up to 2600m2/g, has outstanding heat conductivility (3000W/ (mK) and mechanical property (1060GPa), and at a high speed electron mobility (15000cm2/ (Vs)) under the room temperature.Graphene particular structural characteristic simultaneously makes its a series of character such as electrical conductivity that have perfect quantum tunneling effect, half integral quantum hall effect, never disappear, and has caused the huge interest of scientific circles, and Graphene is just starting the upsurge of one research.
Carbon nano-fiber is solid, the fiber fines shape object of diameter between 50-200nm.Carbon in the carbon fiber is lack of alignment more.See that from crystal structure the carbon nano-fiber crystallization degree that has is very high, defective seldom; But the degree of graphitization that has is very low, even approaches amorphous state.It is found that in recent years carbon nano-fiber has a lot of good characteristics, like high strength, high elastic modulus, high conductivity etc.Carbon fiber has excellent mechanical property, and its intensity and modulus substantially exceed general fibrous materials such as gathering vinegar fiber, glass fibre, superhigh molecular weight polyethylene fibers, silicon carbide fibre and alumina silicate fibre.In addition, carbon fiber also has characteristics such as light weight, high temperature resistant, DIMENSIONAL STABILITY and chemical stability be good.Carbon fiber has the characteristic of " light and strong " and " light and hard ", has obtained to use widely at many high-technology fields such as Aeronautics and Astronautics, automobile, motions.The composite material strength of processing with carbon fiber is high, and is shock-resistant, in light weight, can alleviate the weight of products such as aircraft, airship base automobile greatly, reduces energy resource consumption, thus cutting down cost significantly; Utilize its DIMENSIONAL STABILITY, be applied to universe machinery, radiotelescope and various moulding article; Utilize its fatigue durability, be applied to the blade of helicopter; Utilize its vibration attenuation property, be applied to sound appliances; Utilize its heat-resisting quantity, be applied to aircraft brake sheet and heat-insulating material; Utilize its resistance to chemical reagents, be applied to airtight and watertight padding and filter material; Utilize its electrical characteristic, be applied to electrode material, electromagnetic shielding material, antistatic material; Utilize its living body adaptability, be applied to artificial bone, ligament; Utilize its X one photopermeability, be applied to X one smooth bed board etc.
(3) summary of the invention
The object of the present invention is to provide a kind of nanometer Preparation Method made of paper that contains Graphene.
The objective of the invention is to realize like this: step is following:
Step 1: the natural flake graphite 30g that gets particle diameter≤45 μ m is a raw material, in 80 ℃ of baking ovens oven dry for use after 24 hours, with the dense H of 30ml
2SO
4, 10g K
2S
2O
8, 10g P
2O
5Mix and be placed in the flask, in flask, add the natural flake graphite of particle diameter≤45 μ m that 30g dried, be heated to 80 ℃ oxidation reactions take place down;
Step 2: step 1 is handled natural flake graphite later adopt the hummers method that its oxidation is obtained graphite oxide;
Step 3: the graphite oxide that step 2 is made joins N; In the mixed solution of N-dimethyl methyl phthalein amine and water, under the 100W ultrasonic power, handle 3h, centrifugal 40min under the speed of 4000r.p.m. then; Remove centrifugal sediment, obtain the graphene oxide dispersion liquid;
Step 4: the graphene oxide dispersion liquid that step 3 is made is behind sonicated 30min; Obtain the stable graphene oxide colloidal suspensions of homogeneous; Add the aqueous solution that content is 80% hydrazine hydrate to it then, and, obtain redox graphene at 120 ℃ of following water-bath back flow reaction 4h;
Step 5: the redox graphene that the weighing step 4 makes; Pressing mass ratio 1: 2 mixes with carbon nano-fiber; The mixture of redox graphene and carbon nano-fiber added to making it dissolving in the deionized water, mixture and deionized water are 1: 100, obtain suspension.
Step 6: the suspension that step 5 is obtained carries out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40min, form the suspension that is evenly distributed;
Step 7: the arrangement pressure vessel, be laid on the sieves ultra-fine hole filter membrane is smooth, it is wetting on sieves, to add low amounts of water then; Sealed pressure vessel will be transferred in the pressure vessel through the suspension after the step 6 sonicated; Through air compressor suspension is pressurizeed, pressure is taked low pressure 0.7MPa, and continue 20min pressing time, obtains wetting film;
Step 8: the wetting film that step 7 is made is transferred to drying baker; Bake out temperature is 100 ℃ to 1300 ℃, and initial 5 ℃/min of heating rate is to 100 ℃ of constant temperature 30min; Continuation rises to 1300 ℃ of terminations with 5 ℃/min; Overall process adopts argon shield, sloughs filter membrane, obtains dry, complete nanometer paper.
A kind of nanometer Preparation Method made of paper that contains Graphene of the present invention; Has following advantage: overlap each other between Graphene and the carbon nano-fiber; Can form effective current path; And, improve microwave absorbing property greatly because both linearity and lamella pattern, erratic surface can be reduced surperficial albedo effectively.Along with the content of Graphene in nanometer paper increases, electric conductivity increases, and when containing the 0.6g Graphene in the 1.8g nanometer paper, overall resistivity reaches 0.6 Ω cm, has reached the conducting metal level.The electric conductivity of the nanometer paper that contains Graphene that the present invention synthesizes has improved about three times than original common nanometer paper electric conductivity; The interpolation of Graphene can increase the proportion of goods damageds of nanometer paper material; And the maximum loss rate of pure carbon nanofiber nanometer paper is 94.1%; Wave absorbed crest value reaches 12dB, and the maximum loss rate of nanometer paper is 96.5% behind the interpolation Graphene, and wave absorbed crest value reaches 13dB.
(4) description of drawings
Fig. 1 is the nanometer of the present invention flow chart that is equipped with made of paper;
Fig. 2 is the Graphene electron-microscope scanning figure that makes;
Fig. 3 is carbon nano-fiber electron-microscope scanning figure;
Fig. 4 is nanometer paper electron-microscope scanning figure of the present invention.
(5) specific embodiment
For example the present invention is described further below in conjunction with accompanying drawing.
Embodiment 1: combine Fig. 1, and a kind of nanometer Preparation Method made of paper that contains Graphene of the present invention,
Step is following:
Step 1: the natural flake graphite 30g that takes by weighing particle diameter≤45 μ m is a raw material, in 80 ℃ of baking ovens oven dry for use after 24 hours, with the dense H of 30ml
2SO
4, 10g K
2S
2O
8, 10g P
2O
5Mix and be placed in the flask, in flask, add the graphite that 30g has been dried, be heated to 80 ℃ oxidation reactions take place down;
Step 2: step 1 is handled natural flake graphite later adopt the humers method that its oxidation is obtained graphite oxide;
Step 3: the graphite oxide that step 2 is made joins N; In the mixed solution of N-dimethyl methyl phthalein amine and water, under the 100W ultrasonic power, handle 3h, centrifugal 40min under the speed of 4000r.p.m. then; Remove centrifugal sediment, obtain the graphene oxide dispersion liquid;
Step 4: the graphene oxide dispersion liquid that step 3 is made is behind sonicated 30min; Obtain the stable graphene oxide colloidal suspensions of homogeneous; Add the aqueous solution that content is 80% hydrazine hydrate to it then, and, obtain redox graphene at 120 ℃ of following water-bath back flow reaction 4h;
Step 5: the redox graphene that the weighing step 4 makes; Pressing mass ratio 1: 2 mixes with carbon nano-fiber; The mixture of redox graphene and carbon nano-fiber added to making it dissolving in the deionized water, mixture and deionized water ratio are 1: 100, obtain suspension.
Step 6: the suspension that step 5 is obtained carries out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40min, form the suspension that is evenly distributed;
Step 7: the arrangement pressure vessel, be laid on the sieves ultra-fine hole filter membrane is smooth, it is wetting on sieves, to add low amounts of water then; Sealed pressure vessel will be transferred in the pressure vessel through the suspension after the step 6 sonicated; Through air compressor suspension is pressurizeed, pressure is taked low pressure 0.7MPa, and continue 20min pressing time, obtains wetting film;
Step 8: the wetting film that step 7 is made is transferred to drying baker; Bake out temperature is 100 ℃ to 1300 ℃, and initial 5 ℃/min of heating rate is to 100 ℃ of constant temperature 30min; Continuation rises to 1300 ℃ of terminations with 5 ℃/min; Overall process adopts argon shield, sloughs filter membrane, obtains dry, complete nanometer paper.
Embodiment 2: combine Fig. 2, the preparation of redox graphene:
Taking by weighing particle diameter≤45 μ m natural flake graphite 30g is raw material, for use behind the dry 24h in 80 ℃ of baking ovens.With 30mL H
2SO
4, 10gK
2S
2O
8, 10gP
2O
5Mixture place flask,, add the above-mentioned dried native graphite of 30g.Be heated to 80 ℃, the question response thing becomes fully and stops heating when black-and-blue, is cooled to room temperature and places 6h.Water fully washes, the filtering reaction thing, is neutral until filtrating.At room temperature dried product and dense H after a last step is dried
2SO
4In 0 ℃ of water-bath, slowly add KMnO
4, the control temperature also slowly adds distilled water in flask, keep reaction a period of time.Add distilled water and H at last again
2O
2, mixture becomes glassy yellow by yellowish-brown.With the HCl solution washing, filter above-mentioned product, to remove the part metals ion.Put into the graphite oxide after the watery hydrochloric acid washing in the bag filter; In distilled water, dialyse, the product after will dialysing is then put into centrifuge, centrifugal 40min; Remove a small amount of not oxidized natural graphite particles, the graphite oxide that obtains is viscosity, brown colloid.Get the graphite oxide that 20g makes and be dispersed in respectively in the water that adds dispersant, stir about 20min,, ultrasonic 3h under the 100W ultrasonic power obtains brown dispersion liquid then.4, centrifugal 40min removes centrifugal sediment under the speed of 000r.p.m., finally obtains the dispersion liquid of graphene oxide.Get suspension sonicated 30min in there-necked flask of above-mentioned graphene oxide, adding mass fraction under the vigorous stirring is the aqueous solution of 80% hydrazine hydrate, at 120 ℃ of following water-bath back flow reaction 4h.Stir after reaction is accomplished and be cooled to room temperature, spend deionised water repeatedly, obtain redox graphene.That as shown in Figure 2 is the electron-microscope scanning figure of prepared Graphene.
Embodiment 3: contain the preparation of graphene nano paper:
Take by weighing the 1.8g carbon nano-fiber, add deionized water, deionized water and carbon nano-fiber mass ratio are 100: 1, obtain suspension; Suspension is carried out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension that is evenly distributed, put pressure vessel then in order; With smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, and sealed pressure vessel is transferred to the suspension after the sonicated in the pressure vessel; Through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 4: contain the preparation of graphene nano paper
Take by weighing 0.1g redox graphene and 1.7g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then under the condition of supersonic frequency 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension be evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 5: contain the preparation of graphene nano paper
Take by weighing 0.2g redox graphene and 1.6g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then under the condition of supersonic frequency 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension be evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 6: contain the preparation of graphene nano paper
Take by weighing 0.3g redox graphene and 1.5g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension that is evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 7: contain the preparation of graphene nano paper
Take by weighing 0.4g redox graphene and 1.4g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension that is evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 8: contain the preparation of graphene nano paper
Take by weighing 0.5g redox graphene and 1.3g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension that is evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 9: contain the preparation of graphene nano paper
Take by weighing 0.6g redox graphene and 1.2g carbon nano-fiber respectively, both are mixed, add deionized water, deionized water is 100: 1 with the mixture quality ratio; Obtain suspension, suspension carried out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40 minutes, form the suspension that is evenly distributed; Put pressure vessel then in order, with smooth being laid on the sieves of ultra-fine hole filter membrane, and it is wetting to add low amounts of water, sealed pressure vessel; Suspension after the sonicated is transferred in the pressure vessel, through air compressor to suspension pressurization in the solution, when in the container during no a large amount of moisture content, take out moistening filter membrane with and on nanometer paper; Carefully be transferred to drying baker, bake out temperature is 100 ℃ to 1300 ℃, initial 5 ℃/min of heating rate; To 100 ℃ of constant temperature 30min, continue to rise to 1300 ℃ of terminations with 5 ℃/min, overall process adopts argon shield; Dry, and slough filter membrane, obtain dry, complete nanometer paper.
Embodiment 10: the step that employing Hummers legal system is equipped with graphite oxide is following:
The concentrated sulfuric acid of the 30g natural flake graphite of handling and 5g sodium nitrate and 230mL mixed place flask; Then flask is placed under 0 ℃ of water bath condition, and slowly add 60g potassium permanganate, then it is transferred to 35 ℃ of water-bath 30min; And progressively add the 460mL deionized water; Temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by sepia, adds 2L distilled water and 100ml mass fraction at last again and be 30% hydrogenperoxide steam generator; Centrifugal filtration and cyclic washing filtrate, vacuumize promptly obtains graphite oxide.
Overlap each other between Graphene and the carbon nano-fiber in the prepared nanometer paper of the present invention; Can form effective current path; Improve microwave absorbing property greatly; And along with the content of Graphene in nanometer paper increases, electric conductivity increases, and the nanometer paper electric conductivity that contains Graphene that the present invention synthesizes has improved about three times than original common nanometer paper electric conductivity.The interpolation of Graphene has not only increased the proportion of goods damageds of nanometer paper material but also has strengthened the wave absorbed crest value of nanometer paper.
Claims (1)
1. nanometer Preparation Method made of paper that contains Graphene, it is characterized in that: step is following:
Step 1: the natural flake graphite 30g that gets particle diameter≤45 μ m is a raw material, in 80 ℃ of baking ovens oven dry for use after 24 hours, with the dense H of 30ml
2SO
4, 10g K
2S
2O
8, 10g P
2O
5Mix and be placed in the flask, be heated to 80 ℃ after, in flask, add the natural flake graphite of particle diameter≤45 μ m that 30g dried, be heated to 80 ℃ oxidation reactions take place down;
Step 2: step 1 is handled natural flake graphite later adopt the hummers method that its oxidation is obtained graphite oxide;
Step 3: the graphite oxide that step 2 is made joins N; In the mixed solution of N-dimethyl methyl phthalein amine and water, under the 100W ultrasonic power, handle 3h, centrifugal 40min under the speed of 4000r.p.m. then; Remove centrifugal sediment, obtain the graphene oxide dispersion liquid;
Step 4: the graphene oxide dispersion liquid that step 3 is made is behind sonicated 30min; Obtain the stable graphene oxide colloidal suspensions of homogeneous; Add the aqueous solution that content is 80% hydrazine hydrate to it then, and, obtain redox graphene at 120 ℃ of following water-bath back flow reaction 4h;
Step 5: the redox graphene that the weighing step 4 makes; Pressing mass fraction mixed with carbon nano-fiber than 1: 2; The mixture of redox graphene and carbon nano-fiber added to making it dissolving in the distilled water, mixture and distilled water volume fraction ratio are 1: 100, obtain suspension.
Step 6: the suspension that step 5 is obtained carries out mechanical agitation 15min, then supersonic frequency be under the condition of 30Hz with the ultrasonic dispersion of mixed liquor 40min, form the suspension that is evenly distributed;
Step 7: the arrangement pressure vessel, be laid on the sieves ultra-fine hole filter membrane is smooth, it is wetting on sieves, to add low amounts of water then; To be transferred to through the suspension after the step 6 sonicated in the pressure vessel, sealed pressure vessel pressurizes to suspension through air compressor, and pressure is taked low pressure 0.7MPa, and continue 20min pressing time, obtains wetting film;
Step 8: the wetting film that step 7 is made is transferred to drying baker; Bake out temperature is 100 ℃ to 1300 ℃, and initial 5 ℃/min of heating rate is to 100 ℃ of constant temperature 30min; Continuation rises to 1300 ℃ of terminations with 5 ℃/min; Overall process adopts argon shield, sloughs filter membrane, obtains dry, complete nanometer paper.
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| CN103319734A (en) * | 2012-03-20 | 2013-09-25 | 沈阳航空航天大学 | Method for preparing carbon nanometer paper enhanced conductive polymer matrix composite material |
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