CN106917071A - The preparation method of graphene nano noble metal multiple tube - Google Patents
The preparation method of graphene nano noble metal multiple tube Download PDFInfo
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- CN106917071A CN106917071A CN201710113579.6A CN201710113579A CN106917071A CN 106917071 A CN106917071 A CN 106917071A CN 201710113579 A CN201710113579 A CN 201710113579A CN 106917071 A CN106917071 A CN 106917071A
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Abstract
The invention discloses a kind of preparation method of graphene nano noble metal multiple tube, including：(1) after taking the immersion of wire dust technology, ultrasound in absolute ethyl alcohol is placed in, is then dried；(2) wire of drying is put into chemical vapor depsotition equipment in its superficial growth Graphene, obtains Graphene/metal wire composite structure；(3) graphenic surface in Graphene/metal wire composite structure deposits nano noble metal particles clad；(4) after the composite construction that will be obtained is put into and removes wire in etching liquid, cleaning, drying obtains graphene nano noble metal multiple tube., with operation is simple, repeatability is strong, the characteristics of environmentally safe for preparation method of the invention.The graphene nano noble metal multiple tube that the present invention is provided has excellent mobility, mechanical strength, thermal conductivity and corrosion resistance, it is adaptable to the numerous areas such as microelectronics, transparency electrode, organic electro-optic device, energy-storage battery, multifunctional composite and biomedicine.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of Graphene-nm of gold multiple tube.
Background technology
Graphene is a kind of two-dimentional allotrope of carbon, since the research group of Univ Manchester UK in 2004 is first
Secondary utilization micromechanics stripping method have successfully been obtained after single-layer graphene, and Graphene obtains the extensive pass of various countries researcher
Note.Although other allotropes of carbon such as CNT, fullerene etc. are all similar with Graphene by sp2 hydbridized carbon atoms groups
Into, but in property sides such as mobility, room temperature Hall effect, diracelectron structure, translucency, mechanical strength and thermal conductivities
Face, these allotropes can not match in excellence or beauty with Graphene.Exactly because these tempting speciality, Graphene such as microelectronics,
The numerous areas such as transparency electrode, organic electro-optic device, energy-storage battery, multifunctional composite and biomedicine have wide
Application prospect.[specific visible document：L.Guo et al.J Phys C,2012,116(5):3594.X.Wang et
al.Nano Lett,2008,8:323.K.K.Manga et al.Adv Mater,2012,24:1697.Y.Zhu et
al.Carbon,2010,48:2118.Y.Wang et al.J Phys Chem C,2011,115:23192.Y Wang et
al.J Am Chem Soc,2010,132:9274.]
Publication number CN102586869A discloses a kind of preparation method of three-dimensional grapheme tube, the grapheme tube skeleton material
Material is the organic materials such as Kynoar, polyethylene glycol, polymethylacrylic acid, and above-mentioned material is enhancing grapheme tube machinery by force
While spending, the important parameters such as the electric conductivity of Graphene are undoubtedly also reduced.Additionally, there is document report to use noble metal and nanometer
The compound method of carbon material can effectively lift its electric conductivity.However, not yet having using wire as growth substrate, in gold at present
Category silk table face deposition is obtained Graphene/metal wire composite structure, and then coats noble metal nano particles in graphenic surface, finally
The relevant report of Graphene-nano-noble metal multiple tube is prepared by removing substrate (wire).
The content of the invention
It is an object of the invention to solve at least the above and/or defect, and provide at least will be described later excellent
Point.
In order to realize these purposes of the invention and further advantage, there is provided a kind of Graphene-nano-noble metal is multiple
The preparation method of pipe is closed, is comprised the following steps：
Step one, take wire dust technology immersion removal surface impurity and passivation layer after, be placed in absolute ethyl alcohol ultrasound,
Then dry for standby；
Step 2, the wire that will be dried are put into chemical vapor depsotition equipment in its superficial growth as growth substrate
Graphene, obtains Graphene/metal wire composite structure；
Step 3, the graphenic surface deposition nano noble metal particles clad in Graphene/metal wire composite structure, shape
Into noble metal clad/Graphene/metal wire composite structure；
Step 4, noble metal clad/Graphene/metal wire composite structure be put into remove wire in etching liquid after,
Dried after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, obtain Graphene-nano-noble metal multiple tube.
Preferably, the wire is copper wire or nickel wire, a diameter of 10nm~1cm of the wire, and length is
10nm~1m.
Preferably, the dust technology concentration be 0.001~1mol/L, wire in dust technology soak time be 1s~
60min, a length of 1~60min during ultrasound in absolute ethyl alcohol；The drying is used in air dry oven, dried process temperature
It it is 40~200 DEG C, process time is 0.1~36h.
Preferably, in the step 3, the expensive gold of nanometer is deposited in the graphenic surface of Graphene/metal wire composite structure
Belong to the deposition process of particle clad in magnetron sputtering, hot evaporation, pulsed laser deposition, chemical plating or electrochemical deposition method
Any one；The sedimentation rate for depositing nano noble metal particles clad is 0.1nm/s~10 μm/s, and the noble metal is
Any one or more alloy material being combined into gold, platinum, palladium, titanium, ruthenium, niobium.
Preferably, a diameter of 10nm~1cm of the Graphene-nano-noble metal multiple tube, length is 10nm~1m.
Preferably, in the step 2, in chemical vapor depsotition equipment, wire surface growth Graphene process
Reaction atmosphere is the gaseous mixture of hydrogen and inert gas, on the premise of programming rate is 5~30 DEG C/min, is heated to reaction temperature
800~1500 DEG C of degree, 0~120min of constant temperature after importing carbon source is reacted, is cooled to room temperature, obtains Graphene/wire multiple
Close structure；The carbon source is the mixing of one or more in methanol steam, alcohol vapour, acetone steam, xylene steam；Institute
The flow for stating carbon source is 10~30sccm.
Preferably, in the step 4, etching liquid is liquor potassic permanganate and/or ferric chloride solution.
Preferably, the process of the step 2 is replaced with：Rotation of receiver of the wire that will be dried as electrostatic spinning
Device, is blended with the polymer spin dope electrostatic spinning of graphene oxide to the wire of rotation, while by Graphene
Dispersion liquid ultrasonic atomizatio forms the wire of electrostatic spinning film and graphene coated on the wire of rotation；The step
In four, after wire is removed during noble metal clad/Graphene/metal wire composite structure is put into etching liquid, N is added into,
12h is soaked in dinethylformamide or toluene, is dried after then being cleaned to products therefrom with absolute ethyl alcohol and deionized water, obtained
Obtain Graphene-nano-noble metal multiple tube.
Preferably, the polymer spin dope is PLA solution, PMA solution, polyimide solution
In one kind；The concentration of the polymer spin dope is 5~10wt%；The graphene oxide and polymer spin dope
Mass ratio is 1：50~100；The graphene oxide is with the mixed process of polymer spin dope：By graphene oxide with it is poly-
Compound spinning solution mixes, and is subsequently adding dispersant 1- ethyl -3- methylimidazolium chlorides, and low whipping speed is 500r/min conditions
Under, mixed solution is heated to 50 DEG C, its reaction 24h is kept, room temperature is cooled to, obtain being mixed with the polymer of graphene oxide
Spinning solution；The dispersant 1- ethyl -3- methylimidazolium chlorides are 1 with the weight ratio of graphene oxide:5~10；
The graphene dispersing solution includes the raw material of following weight portion：10~15 parts of Graphene, 1- ethyl-3-methylimidazoles
1~3 part of lactic acid, 30~50 parts of cyclohexanone, 30~50 parts of N- cyclohexyl pyrrolidones, 30~50 parts of propandiol butyl ether acetate.
Preferably, the electrospinning process is：It is blended with the polymer spin dope injection band of graphene oxide
In the spray containers of stainless steel shower nozzle, then applied the voltage on stainless steel shower nozzle with high voltage power supply, and held using with injection
The propulsion pump of device connection connects the polymer spin dope in spray containers by the wire that stainless steel shower nozzle is sprayed to rotation
On receiving apparatus, the injection conditions of the electrostatic spinning is：Environment temperature is 40~80 DEG C, the output voltage of high voltage power supply for 15~
Distance is that 10~15cm, flow velocity are 5~12mL/h, the rotation of wire reception device between 25kv, wire and stainless steel shower nozzle
Rotary speed is 50~500r/min；
The power of the graphene dispersing solution ultrasonic atomizatio is 80W, and frequency is 2.5MHz, and condensation rate is 2~10mL/min,
The ejiction opening of ultrasonic atomizatio is 5~15cm with the distance of wire..
The present invention at least includes following beneficial effect：Preparation method of the invention is repeatable with operation is simple
By force, environmentally safe the characteristics of.Graphene-nano-noble metal multiple tube that the present invention is provided has excellent mobility, machine
Tool intensity, thermal conductivity and corrosion resistance, it is adaptable to microelectronics, transparency electrode, organic electro-optic device, energy-storage battery, multi-functional multiple
The numerous areas such as condensation material and biomedicine.
Further advantage of the invention, target and feature embody part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings：
Fig. 1 is the ESEM of the noble metal clad/Graphene/copper wire composite construction of preparation in the embodiment of the present invention 1
Photo (a) sweeps result with the EDS of correspondence position into facet, is respectively carbon (b), copper (c) and gold (d)；
Fig. 2 is the EDS faces score of the noble metal clad/Graphene/copper wire composite construction of preparation in the embodiment of the present invention 1
Figure；
Fig. 3 is the light microscope sectional view of the Graphene-nano-noble metal multiple tube of preparation in the embodiment of the present invention 1.
Specific embodiment：
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that it is used herein such as " have ", "comprising" and " including " term do not allot one or many
The presence or addition of individual other elements or its combination.、
Embodiment 1：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, take 15 μm of diameter, the copper wire of length 5cm soaks 2min and removes surface impurity with the dust technology of 0.1mol/L
And after passivation layer, ultrasound 20min in absolute ethyl alcohol is placed in, it is then placed into 60 DEG C of drying 2h dry for standby in air dry oven；
Step 2, the copper wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 30 DEG C/min, 1000 DEG C are heated to, constant temperature 60min is passed through alcohol vapour
10sccm is reacted, and reaction stops being passed through alcohol vapour after terminating, and is quickly cooled to room temperature, obtains Graphene/copper wire and is combined
Structure；
Step 3, by magnetron sputtering method, under conditions of deposition velocity is 20nm/s, in obtained Graphene/copper wire
Composite structure surface deposits nm of gold clad, forms nm of gold clad/Graphene/copper wire composite construction；Fig. 1 shows and receives
Golden clad/Graphene/the scanning electron microscope (SEM) photograph (a) of copper wire composite construction of rice sweeps result with the EDS of correspondence position into facet, respectively
It is carbon (b), copper (c) and gold (d)；Fig. 2 shows the total spectrogram in EDS faces of nm of gold clad/Graphene/copper wire composite construction；
Step 4, nm of gold clad/Graphene/copper wire composite construction is put into iron chloride etching liquid and removes copper wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-nm of gold multiple tube；Fig. 3 shows the optics of Graphene-nano metal multiple tube after present invention removal growth substrate copper wire
Microscope sectional view.
Embodiment 2：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, take 15 μm of diameter, the nickel wire of length 5cm soaks 2min and removes surface impurity with the dust technology of 0.1mol/L
And after passivation layer, ultrasound 20min in absolute ethyl alcohol is placed in, it is then placed into 60 DEG C of drying 2h dry for standby in air dry oven；
Step 2, the nickel wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 30 DEG C/min, 1000 DEG C are heated to, constant temperature 60min is passed through alcohol vapour
10sccm is reacted, and reaction stops being passed through alcohol vapour after terminating, and is quickly cooled to room temperature, obtains graphene/nickel silk compound
Structure；
Step 3, by magnetron sputtering method, under conditions of deposition velocity is 20nm/s, in obtained graphene/nickel silk
Composite structure surface deposits nm of gold clad, forms nm of gold clad/graphene/nickel filament composite structure；
Step 4, nm of gold clad/graphene/nickel filament composite structure is put into iron chloride etching liquid removes copper wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-nm of gold multiple tube.
Embodiment 3：
The preparation method of a kind of Graphene-nano-noble metal multiple tube, it is characterised in that comprise the following steps：
Step one, take 15 μm of diameter, the copper wire of length 5cm soaks 2min and removes surface impurity with the dust technology of 0.1mol/L
And after passivation layer, ultrasound 20min in absolute ethyl alcohol is placed in, it is then placed into 60 DEG C of drying 2h dry for standby in air dry oven；
Step 2, the copper wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 20 DEG C/min, 1050 DEG C are heated to, constant temperature 30min is passed through alcohol vapour
20sccm is reacted, and reaction stops being passed through alcohol vapour after terminating, and is quickly cooled to room temperature, obtains Graphene/copper wire and is combined
Structure；
Step 3, by magnetron sputtering method, under conditions of deposition velocity is 20nm/s, in obtained Graphene/copper wire
Composite structure surface deposits nm of gold clad, forms nm of gold clad/Graphene/copper wire composite construction；
Step 4, nm of gold clad/Graphene/copper wire composite construction is put into iron chloride etching liquid and removes copper wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-nm of gold multiple tube.
Embodiment 4：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, take 15 μm of diameter, the copper wire of length 5cm soaks 2min and removes surface impurity with the dust technology of 0.1mol/L
And after passivation layer, ultrasound 20min in absolute ethyl alcohol is placed in, it is then placed into 60 DEG C of drying 2h dry for standby in air dry oven；
Step 2, the copper wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 30 DEG C/min, 1000 DEG C are heated to, constant temperature 60min is passed through alcohol vapour
10sccm is reacted, and reaction stops being passed through alcohol vapour after terminating, and is quickly cooled to room temperature, obtains Graphene/copper wire and is combined
Structure；
Step 3, by chemical plating method, in obtained Graphene/copper wire composite structure surface deposition nm of gold cladding
Layer, forms nm of gold clad/Graphene/copper wire composite construction；
Step 4, nm of gold clad/Graphene/copper wire composite construction is put into iron chloride etching liquid and removes copper wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-nm of gold multiple tube.
Embodiment 5：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, the nickel wire for taking 30 μm of diameter, length 10cm soak 20min to remove surface miscellaneous with the dust technology of 0.5mol/L
After matter and passivation layer, ultrasound 30min in absolute ethyl alcohol is placed in, is then placed into 100 DEG C of drying 1h drying in air dry oven standby
With；
Step 2, the nickel wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 15 DEG C/min, 1200 DEG C are heated to, constant temperature 30min is passed through acetone steam
30sccm is reacted, and reaction stops being passed through acetone steam after terminating, and is quickly cooled to room temperature, obtains graphene/nickel silk compound
Structure；
Step 3, by pulse laser sediment method, deposit nm of gold on obtained graphene/nickel filament composite structure surface
Clad, forms nm of gold clad/graphene/nickel filament composite structure；
Step 4, nm of gold clad/graphene/nickel filament composite structure is put into potassium permanganate etching liquid removes nickel wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-nm of gold multiple tube.
Embodiment 6：
The preparation method of a kind of Graphene-nano-noble metal multiple tube, it is characterised in that comprise the following steps：
Step one, the copper wire for taking 50 μm of diameter, length 10cm soak 10min to remove surface miscellaneous with the dust technology of 0.5mol/L
After matter and passivation layer, ultrasound 30min in absolute ethyl alcohol is placed in, is then placed into 80 DEG C of drying 2h drying in air dry oven standby
With；
Step 2, the copper wire that will be dried are put into chemical vapor depsotition equipment as growth substrate, and reaction atmosphere is hydrogen
With the gaseous mixture of nitrogen, under the programming rate of 10 DEG C/min, 1500 DEG C are heated to, constant temperature 100min is passed through xylene steam
20sccm is reacted, and reaction stops being passed through xylene steam after terminating, and is quickly cooled to room temperature, obtains Graphene/copper wire multiple
Close structure；
Step 3, by electrochemical deposition method, in obtained Graphene/copper wire composite structure surface deposition Technique of Nano Pd bag
Coating, forms Technique of Nano Pd clad/Graphene/copper wire composite construction；
Step 4, Technique of Nano Pd clad/Graphene/copper wire composite construction is put into iron chloride etching liquid and removes copper wire
Afterwards, 60 DEG C of drying 2h in air dry oven are positioned over after being cleaned to products therefrom with absolute ethyl alcohol and deionized water, graphite is obtained
Alkene-Technique of Nano Pd multiple tube.
Embodiment 7：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, the copper wire for taking 50 μm of diameter, length 10cm soak 10min to remove surface miscellaneous with the dust technology of 0.5mol/L
After matter and passivation layer, ultrasound 30min in absolute ethyl alcohol is placed in, is then placed into 80 DEG C of drying 2h drying in air dry oven standby
With；
Step 2, the copper wire that will be dried are blended with the poly- of graphene oxide as the Rotation of receiver device of electrostatic spinning
Compound spinning solution electrostatic spinning to rotation copper wire on, while by graphene dispersing solution ultrasonic atomizatio in rotation copper wire on,
Form the copper wire of electrostatic spinning film and graphene coated；
Step 3, by electrochemical deposition method, be combined in the copper wire of obtained electrostatic spinning film and graphene coated
Body structure surface deposits Platinum Nanoparticles clad；
Step 4, the composite construction that step 3 is obtained be put into remove copper wire in iron chloride etching liquid after, be added into N,
12h is soaked in dinethylformamide or toluene, is positioned over after then being cleaned to products therefrom with absolute ethyl alcohol and deionized water
60 DEG C of drying 2h, obtain Graphene-Platinum Nanoparticles multiple tube in air dry oven；
Wherein, the polymer spin dope is PLA solution；The concentration of the polymer spin dope is 5wt%；
The graphene oxide is 1 with the mass ratio of polymer spin dope：50；The graphene oxide and polymer spin dope
Mixed process is：Graphene oxide is mixed with polymer spin dope, dispersant 1- ethyl -3- methyl chloride miaows are subsequently adding
Azoles, low whipping speed keeps its reaction 24h under the conditions of 500r/min, mixed solution to be heated into 50 DEG C, is cooled to room temperature,
Obtain being mixed with the polymer spin dope of graphene oxide；The dispersant 1- ethyl -3- methylimidazolium chlorides and oxidation stone
The weight ratio of black alkene is 1:5；The graphene dispersing solution includes the raw material of following weight portion：10 parts of Graphene, 1- ethyl -3- first
1 part of base imidazole lactic acid, 30 parts of cyclohexanone, 30 parts of N- cyclohexyl pyrrolidones, 30 parts of propandiol butyl ether acetate；
The electrospinning process is：It is blended with the polymer spin dope injection band stainless steel shower nozzle of graphene oxide
Spray containers in, then applied the voltage on stainless steel shower nozzle with high voltage power supply, and using pushing away of being connected with spray containers
Enter pump to spray to the wire reception device of rotation the polymer spin dope in spray containers by stainless steel shower nozzle, institute
The injection conditions for stating electrostatic spinning is：Environment temperature is 40 DEG C, the output voltage of high voltage power supply is 15kv, wire and stainless steel
Between shower nozzle distance be 10cm, flow velocity be 5mL/h, wire reception device rotary speed be 50r/min；
The power of the graphene dispersing solution ultrasonic atomizatio is 80W, and frequency is 2.5MHz, and condensation rate is 2mL/min, ultrasound
The ejiction opening of atomization is 5cm with the distance of wire.
Embodiment 8：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, the copper wire for taking diameter 1cm, length 30cm soak 10min to remove surface miscellaneous with the dust technology of 0.5mol/L
After matter and passivation layer, ultrasound 30min in absolute ethyl alcohol is placed in, is then placed into 80 DEG C of drying 2h drying in air dry oven standby
With；
Step 2, the copper wire that will be dried are blended with the poly- of graphene oxide as the Rotation of receiver device of electrostatic spinning
Compound spinning solution electrostatic spinning to rotation copper wire on, while by graphene dispersing solution ultrasonic atomizatio in rotation copper wire on,
Form the copper wire of electrostatic spinning film and graphene coated；
Step 3, by magnetically controlled sputter method, in obtained electrostatic spinning film and the copper wire composite junction of graphene coated
Structure surface deposits nano-titanium clad；
Step 4, the composite construction that step 3 is obtained be put into remove copper wire in iron chloride etching liquid after, be added into N,
12h is soaked in dinethylformamide or toluene, is positioned over after then being cleaned to products therefrom with absolute ethyl alcohol and deionized water
60 DEG C of drying 2h, obtain Graphene-nanometer composite ti pipe in air dry oven；
Wherein, the polymer spin dope is PMA solution；The concentration of the polymer spin dope is
10wt%；The graphene oxide is 1 with the mass ratio of polymer spin dope：100；The graphene oxide and polymer spun
The mixed process of silk stock solution is：Graphene oxide is mixed with polymer spin dope, dispersant 1- ethyl -3- first is subsequently adding
Base imidazolitm chloride, low whipping speed keeps its reaction 24h, cooling under the conditions of 500r/min, mixed solution to be heated into 50 DEG C
To room temperature, obtain being mixed with the polymer spin dope of graphene oxide；The dispersant 1- ethyl -3- methylimidazolium chlorides with
The weight ratio of graphene oxide is 1:10；The graphene dispersing solution includes the raw material of following weight portion：15 parts of Graphene, 1- second
3 parts of base -3- methylimidazoles lactic acid, 50 parts of cyclohexanone, 50 parts of N- cyclohexyl pyrrolidones, 50 parts of propandiol butyl ether acetate；
The electrospinning process is：It is blended with the polymer spin dope injection band stainless steel shower nozzle of graphene oxide
Spray containers in, then applied the voltage on stainless steel shower nozzle with high voltage power supply, and using pushing away of being connected with spray containers
Enter pump to spray to the wire reception device of rotation the polymer spin dope in spray containers by stainless steel shower nozzle, institute
The injection conditions for stating electrostatic spinning is：Environment temperature is 80 DEG C, the output voltage of high voltage power supply is 25kv, wire and stainless steel
Between shower nozzle distance be 15cm, flow velocity be 12mL/h, wire reception device rotary speed be 500r/min；
The power of the graphene dispersing solution ultrasonic atomizatio is 80W, and frequency is 2.5MHz, and condensation rate is 10mL/min, is surpassed
The ejiction opening of sound atomization is 15cm with the distance of wire.
Embodiment 9：
A kind of preparation method of Graphene-nano-noble metal multiple tube, comprises the following steps：
Step one, the nickel wire for taking diameter 0.5cm, length 20cm soak 10min to remove surface miscellaneous with the dust technology of 1mol/L
After matter and passivation layer, ultrasound 60min in absolute ethyl alcohol is placed in, is then placed into 80 DEG C of drying 2h drying in air dry oven standby
With；
Step 2, the nickel wire that will be dried are blended with the poly- of graphene oxide as the Rotation of receiver device of electrostatic spinning
Compound spinning solution electrostatic spinning to rotation nickel wire on, while by graphene dispersing solution ultrasonic atomizatio in rotation nickel wire on,
Form the nickel wire of electrostatic spinning film and graphene coated；
Step 3, by magnetically controlled sputter method, in obtained electrostatic spinning film and the nickel wire composite junction of graphene coated
Structure surface deposits nm of gold clad；
Step 4, the composite construction that step 3 is obtained be put into remove nickel wire in iron chloride etching liquid after, be added into N,
12h is soaked in dinethylformamide or toluene, is positioned over after then being cleaned to products therefrom with absolute ethyl alcohol and deionized water
60 DEG C of drying 2h, obtain Graphene-nm of gold multiple tube in air dry oven；
Wherein, the polymer spin dope is polyimide solution；The concentration of the polymer spin dope is
10wt%；The graphene oxide is 1 with the mass ratio of polymer spin dope：60；The graphene oxide and polymer spun
The mixed process of silk stock solution is：Graphene oxide is mixed with polymer spin dope, dispersant 1- ethyl -3- first is subsequently adding
Base imidazolitm chloride, low whipping speed keeps its reaction 24h, cooling under the conditions of 500r/min, mixed solution to be heated into 50 DEG C
To room temperature, obtain being mixed with the polymer spin dope of graphene oxide；The dispersant 1- ethyl -3- methylimidazolium chlorides with
The weight ratio of graphene oxide is 1:8；The graphene dispersing solution includes the raw material of following weight portion：12 parts of Graphene, 1- second
2 parts of base -3- methylimidazoles lactic acid, 40 parts of cyclohexanone, 40 parts of N- cyclohexyl pyrrolidones, 40 parts of propandiol butyl ether acetate；
The electrospinning process is：It is blended with the polymer spin dope injection band stainless steel shower nozzle of graphene oxide
Spray containers in, then applied the voltage on stainless steel shower nozzle with high voltage power supply, and using pushing away of being connected with spray containers
Enter pump to spray to the wire reception device of rotation the polymer spin dope in spray containers by stainless steel shower nozzle, institute
The injection conditions for stating electrostatic spinning is：Environment temperature is 60 DEG C, the output voltage of high voltage power supply is 20kv, wire and stainless steel
Between shower nozzle distance be 12cm, flow velocity be 8mL/h, wire reception device rotary speed be 150r/min；
The power of the graphene dispersing solution ultrasonic atomizatio is 80W, and frequency is 2.5MHz, and condensation rate is 5mL/min, ultrasound
The ejiction opening of atomization is 10cm with the distance of wire.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and implementation method
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the legend with description.
Claims (10)
1. the preparation method of a kind of Graphene-nano-noble metal multiple tube, it is characterised in that comprise the following steps：
Step one, take wire dust technology immersion removal surface impurity and passivation layer after, be placed in absolute ethyl alcohol ultrasound, then
Dry for standby；
Step 2, the wire that will be dried are put into chemical vapor depsotition equipment in its superficial growth graphite as growth substrate
Alkene, obtains Graphene/metal wire composite structure；
Step 3, the graphenic surface deposition nano noble metal particles clad in Graphene/metal wire composite structure, form expensive
Metal carbonyl coat/Graphene/metal wire composite structure；
Step 4, noble metal clad/Graphene/metal wire composite structure be put into remove wire in etching liquid after, with nothing
Water-ethanol and deionized water are dried after being cleaned to products therefrom, obtain Graphene-nano-noble metal multiple tube.
2. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the metal
Silk is copper wire or nickel wire, and a diameter of 10nm~1cm of the wire, length is 10nm~1m.
3. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that dilute nitre
Acid concentration is 0.001~1mol/L, and wire soak time in dust technology is 1s~60min, in absolute ethyl alcohol during ultrasound
A length of 1~60min；Using in air dry oven, dried process temperature is 40~200 DEG C, and process time is 0.1 for the drying
~36h.
4. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the step
In three, the deposition process for depositing nano noble metal particles clad in the graphenic surface of Graphene/metal wire composite structure is
Any one in magnetron sputtering, hot evaporation, pulsed laser deposition, chemical plating or electrochemical deposition method；The deposition expensive gold of nanometer
The sedimentation rate for belonging to particle clad is 0.1nm/s~10 μm/s, and the noble metal is any in gold, platinum, palladium, titanium, ruthenium, niobium
The alloy material being combined into for one or more.
5. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the graphite
A diameter of 10nm~1cm of alkene-nano-noble metal multiple tube, length is 10nm~1m.
6. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the step
In two, in chemical vapor depsotition equipment, the reaction atmosphere of wire surface growth Graphene process is hydrogen and inert gas
Gaseous mixture, on the premise of programming rate is 5~30 DEG C/min, be heated to 800~1500 DEG C of reaction temperature, constant temperature 0~
120min, after importing carbon source is reacted, is cooled to room temperature, obtains Graphene/metal wire composite structure；The carbon source is methyl alcohol
One or more in steam, alcohol vapour, acetone steam, xylene steam of mixing；The flow of the carbon source be 10~
30sccm。
7. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the step
In four, etching liquid is liquor potassic permanganate and/or ferric chloride solution.
8. the preparation method of Graphene as claimed in claim 1-nano-noble metal multiple tube, it is characterised in that the step
Two process is replaced with：The wire that will be dried is blended with graphene oxide as the Rotation of receiver device of electrostatic spinning
Polymer spin dope electrostatic spinning to rotation wire on, while by graphene dispersing solution ultrasonic atomizatio in rotation metal
On silk, the wire of electrostatic spinning film and graphene coated is formed；In the step 4, noble metal clad/Graphene/
Metal wire composite structure is put into after removing wire in etching liquid, is added into being soaked in DMF or toluene
12h, dries after then being cleaned to products therefrom with absolute ethyl alcohol and deionized water, obtains Graphene-nano-noble metal multiple tube.
9. the preparation method of Graphene as claimed in claim 8-nano-noble metal multiple tube, it is characterised in that the polymerization
Thing spinning solution is the one kind in PLA solution, PMA solution, polyimide solution；The polymer spinning is former
The concentration of liquid is 5~10wt%；The graphene oxide is 1 with the mass ratio of polymer spin dope：50~100；The oxygen
Graphite alkene is with the mixed process of polymer spin dope：Graphene oxide is mixed with polymer spin dope, Ran Houjia
Enter dispersant 1- ethyl -3- methylimidazolium chlorides, under the conditions of low whipping speed is 500r/min, mixed solution is heated to 50
DEG C, its reaction 24h is kept, room temperature is cooled to, obtain being mixed with the polymer spin dope of graphene oxide；The dispersant 1-
Ethyl -3- methylimidazolium chlorides are 1 with the weight ratio of graphene oxide:5~10；
The graphene dispersing solution includes the raw material of following weight portion：10~15 parts of Graphene, 1- ethyl-3-methylimidazole lactic acid
1~3 part, 30~50 parts of cyclohexanone, 30~50 parts of N- cyclohexyl pyrrolidones, 30~50 parts of propandiol butyl ether acetate.
10. the preparation method of Graphene as claimed in claim 8-nano-noble metal multiple tube, it is characterised in that the electrostatic
Spinning process is：It is blended with the polymer spin dope of graphene oxide spray containers of the injection with stainless steel shower nozzle, so
Applied the voltage on stainless steel shower nozzle with high voltage power supply afterwards, and using the propulsion pump being connected with spray containers by spray containers
Polymer spin dope by stainless steel shower nozzle spray to rotation wire reception device on, the injection of the electrostatic spinning
Condition is：Environment temperature is 40~80 DEG C, the output voltage of high voltage power supply is between 15~25kv, wire and stainless steel shower nozzle
Distance for 10~15cm, flow velocity be 5~12mL/h, wire reception device rotary speed be 50~500r/min；
The power of the graphene dispersing solution ultrasonic atomizatio is 80W, and frequency is 2.5MHz, and condensation rate is 2~10mL/min, ultrasound
The ejiction opening of atomization is 5~15cm with the distance of wire.
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