CN102942178A - Compound base of precious metal nanometer array and single layer graphene and preparation method thereof - Google Patents
Compound base of precious metal nanometer array and single layer graphene and preparation method thereof Download PDFInfo
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- CN102942178A CN102942178A CN2012104768618A CN201210476861A CN102942178A CN 102942178 A CN102942178 A CN 102942178A CN 2012104768618 A CN2012104768618 A CN 2012104768618A CN 201210476861 A CN201210476861 A CN 201210476861A CN 102942178 A CN102942178 A CN 102942178A
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Abstract
The invention discloses a compound base of a precious metal nanometer array and single layer graphene and a preparation method thereof. The invention includes transferring the single layer graphene prepared by a chemical vapor deposition method to the precious metal nanometer array, keeping warm for 30 minutes under the temperature of 50 DEG C, firmly combining the single layer graphene and the precious metal nanometer array to form the compound base of the precious metal nanometer array and the single layer graphene. The preparation method is simple and easy to operate and low in raw material price. The obtained compound base is order in large area. The compound base can be applied to photoelectron devices and the fields of surface enhanced raman chips, thin film solar batteries and the like.
Description
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Technical field
The invention belongs to field of nanometer material technology, relate in particular to a kind of noble metal nano array and single-layer graphene composite substrate and preparation method thereof.
Background technology
Graphene is a kind of Novel Carbon Nanomaterials, be the monoatomic layer material with bi-dimensional cellular shape structure take phenyl ring as elementary cell that is made of carbon atom, it is the elementary cell that makes up other dimension carbonaceous materials (such as zero dimension soccerballene, one dimension carbon nanotube, three-dimensional graphite etc.).Because the structure of Graphene uniqueness and excellent optics, electricity, thermal property, be expected to be applied to high speed transistor, transparency electrode, solar cell, receive the fields such as Mechatronic Systems (NEMS) device, matrix material, catalytic material gas sensor and atmosphere storage.Therefore, Graphene becomes rapidly chemistry, Materials science and Condensed Matter Physics field study hotspot in recent years, has very strong development and application and is worth.
In order further to improve the performance of Graphene, it is compound usually to adopt Graphene and other nano materials to carry out, and the performance of nano material also can be improved simultaneously.The preparation method of existing Graphene composite nano materials mainly contains following several: (1) graft process, yields poorly, generally as fundamental research at the method poor controllability; (2) blending method is usually used in Graphene and polymkeric substance is compound, by making matrix material after polymkeric substance and the blend of graphene nano particle, still is difficult to obtain the matrix material of big area, thickness homogeneous; (3) sol-gel method graphene film is mixed rear preparation matrix material with metal oxide sol, but the method can be destroyed Graphene plane carbon skeleton, produces defective, causes the Graphene degradation.Therefore, how simply controllably preparing large-area ordered and the not obvious graphene composite material that increases of Graphene defective, is large difficult point and a focus of studying at present.
Summary of the invention
For having problems among the existing graphene composite material preparation method, the present invention proposes a kind of simple controlled noble metal nano array and the preparation method of single-layer graphene composite substrate, adopt the method can prepare large-area ordered and the not obvious noble metal nano array that increases of Graphene defective and single-layer graphene composite substrate.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
One, a kind of noble metal nano array and single-layer graphene composite substrate, comprise single-layer graphene layer and noble metal nano array layer, described noble metal nano array layer comprises Cr nanometer thin rete and noble metal nano thin film layer, Cr nano thin-film layer thickness is 10 nm, the noble metal film layer is Ag nanometer thin rete, and its thickness is 60nm.
Two, a kind of method for preparing noble metal nano array and single-layer graphene composite substrate comprises step:
Step 1 adopts Vacuum Coating method to prepare the noble metal nano array;
Step 2 adopts chemical Vapor deposition process to prepare single-layer graphene;
Step 3 is transferred to step 2 gained single-layer graphene on the step 1 gained noble metal nano array, obtains noble metal nano array and single-layer graphene composite substrate.
Above-mentioned steps one is specially:
1.1 adopt the liquid level self-assembly method at self-assembly substrate preparation nanometer ball mask plate; Described self-assembly substrate is preferably silicon chip, and described nanometer ball mask plate is preferably the polystyrene nanospheres mask plate, and the polystyrene nanospheres diameter is 460～800nm;
1.2 utilize Vacuum Coating method to plate successively Cr nano thin-film, noble metal nano film on the nanometer ball mask plate, the Cr nano film thickness that plates is 10 nm, the noble metal nano film that plates is preferably the Ag nano thin-film, and its thickness is 60nm;
1.3 remove the nanometer ball mask plate, obtain the noble metal nano array.
Be to adopt thermal evaporation plating method successively evaporation Cr nano thin-film, noble metal nano film on the nanometer ball mask plate in the above-mentioned steps 1.2, the Cr nano thin-film is used for strengthening the sticking power of noble metal nano film and substrate.
Above-mentioned steps two is specially:
2.1 adopt chemical mechanical polishing method to process metal base, metal base is preferably the Cu paper tinsel;
2.2 adopt chemical Vapor deposition process deposited monolayers Graphene on metal base, selection process is: single-layer graphene is at CH
4And H
2Mixed-gas atmosphere in grow CH
4And H
2Flow be respectively 35sccm and 6sccm, growth temperature is 1020 ℃;
2.3 apply glue-line at single-layer graphene, glue-line is preferably polymetylmethacrylate;
2.4 the substrate of employing chemical etching method corroding metal obtains the single-layer graphene with glue-line.
Above-mentioned steps 2.3 is specially: at single-layer graphene surface-coated polymetylmethacrylate and be heating and curing.
Above-mentioned steps 2.4 is specially: the single-layer graphene with metal base that step 2.3 is obtained places ferric chloride Solution to erode the Cu paper tinsel.
Above-mentioned steps three is specially:
3.1 the single-layer graphene of step 2.4 gained with glue-line is transferred on the noble metal nano array after cleaning, to dry, the selection process of oven dry is: insulation is 30 minutes under 50 ℃;
3.2 remove glue-line after the oven dry, dry up through nitrogen, obtain noble metal nano array and single-layer graphene composite substrate.
When glue-line is polymetylmethacrylate, adopt acetone soln dissolving polymethylmethacrylate to remove polymethylmethacrylate.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1) the present invention when improving conventional surface enhancing Raman scattering substrate homogeneity, stability, poor repeatability, improves the enhancement factor of GENERS by making up metal nano array and single-layer graphene composite strengthening substrate (GENERS).The GENERS substrate that the present invention proposes has following advantage and application: 1. signal is true: the interference such as molecule side reaction of the direct molecular structure deformation that contacts the chemisorption key chattering that produces, metal inducement that the GENERS substrate can isolating metal-probe, metal-probe molecule charge transfer, metal catalytic; 2. signal stabilization: Graphene-molecule forms stable compound easily, thereby can be avoided or weaken in the GENERS system; 3. can be used as fluorescence quenching and natural interior mark: thus graphene layer can disturb by cancellation fluorescence Fluorophotometry; 4. cycle detection: the Graphene sealing coat of inertia has effectively stoped the strong interaction of probe-metal, and under the felicity condition, GENERS substrate of the present invention realizes " detecting-cleaning-detect " circulation easily.
2) it is large-area ordered that the inventive method adopts the noble metal nano array of liquid level extraction method preparation, and low for equipment requirements; The present invention adopts the chemical vapor deposition (CVD) technology to prepare big area individual layer high-quality graphene in metal base; The inventive method is transferred to the treated composite substrate that obtains single-layer graphene and precious metal array firm attachment on the noble metal nano array with the single-layer graphene on the metal base, and complex method is simple to operation, and the gained composite substrate is large-area ordered.
3) the inventive method gained composite substrate can be applicable to opto-electronic device, such as surface-enhanced Raman chip, the fields such as thin-film solar cells.
Description of drawings
Fig. 1 is scanning electronic microscope (SEM) picture of embodiment 1 prepared composite substrate;
Fig. 2 is Raman (Raman) the spectrum picture of embodiment 1 prepared composite substrate;
Fig. 3 is scanning electronic microscope (SEM) picture of embodiment 2 prepared composite substrate;
Fig. 4 is Raman (Raman) the spectrum picture of embodiment 2 prepared composite substrate.
Embodiment
The specific implementation process of the inventive method is as follows:
Step 1 utilizes vacuum plating unit to prepare the noble metal nano array.
At first, be the polystyrene nanospheres mask plate that the individual layer of 460～800nm is closely arranged by the liquid level self-assembly method at the smart silicon chip preparation diameter of throwing of single face; Then, utilize vacuum plating unit, the Ag film of the Cr film of evaporation 10 nm, 60 nm obtains substrate successively on the polystyrene nanospheres mask plate, and the sedimentation rate of Cr film and Ag film is 3 nm/min; Then, substrate is placed chloroform ultrasonic 20 seconds, left standstill 10 minutes, remove the polystyrene nanospheres mask plate and obtain the noble metal nano array; At last, the noble metal nano array is cleaned in alcohol, deionized water successively.
Step 2 adopts chemical Vapor deposition process to prepare single-layer graphene.
At first, adopt chemical mechanical polishing method to process metal base Cu paper tinsel, guarantee that Cu paper tinsel surface clean is smooth, the Cu paper tinsel thickness that adopts is 25 μ m; Then, adopt chemical Vapor deposition process deposited monolayers Graphene on the Cu paper tinsel of processing, selection process is: single-layer graphene is at CH
4And H
2Mixed-gas atmosphere in grow CH
4And H
2Flow be respectively 35sccm and 6sccm, growth temperature is 1020 ℃; Then, apply polymetylmethacrylate at single-layer graphene, through being heating and curing, curing process is: insulation is 30 minutes under 120 ℃; At last, employing ferric chloride Solution corrosion Cu paper tinsel obtains the single-layer graphene with polymethyl methacrylate layers.
Step 3 is transferred to step 2 gained single-layer graphene on the step 1 gained noble metal nano array, namely forms noble metal nano array and single-layer graphene composite substrate.
At first, the employing hydrochloric acid cleaning is coated with the single-layer graphene with polymethyl methacrylate layers, uses washed with de-ionized water 8～10 times again, guarantees iron ion is cleaned up; Then, the single-layer graphene after cleaning is transferred on the noble metal nano array, and dried in 30 minutes 50 ℃ of lower insulations; Then, adopt acetone soln dissolving polymethylmethacrylate; At last, dry up through nitrogen, single-layer graphene just with noble metal nano array mortise, namely obtain noble metal nano array and single-layer graphene composite substrate.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
Throwing on the monocrystalline silicon piece in the single face essence, is that the polystyrene nanospheres of 460 nm makes the mask plate that individual layer is closely arranged by the liquid level self-assembly method with diameter.Utilize vacuum plating unit, the Cr film of first evaporation 10 nm thickness, the Ag film of evaporation 60 nm thickness again obtain substrate on the polystyrene nanospheres mask plate.With substrate in chloroform ultrasonic 20 seconds, left standstill 10 minutes, remove polystyrene microsphere and obtain the Ag nano-array, and in alcohol, deionized water, clean up successively.
Adopting chemical mechanical polishing method to process thickness is the Cu paper tinsel of 25 μ m, smooth to guarantee Cu paper tinsel surface clean; Again under 1020 ℃, in methane and hydrogen mixed gas atmosphere, adopt chemical Vapor deposition process at the Cu paper tinsel of the processing single-layer graphene of growing, in the Graphene process of growth, the flow of methane and hydrogen is controlled to be respectively 35sccm and 6sccm.At the single-layer graphene surface-coated PMMA layer of growing, be cured in 30 minutes in 120 ℃ of lower insulations, then be put into ferric chloride Solution with the corrosion of corrosion Cu paper tinsel.
After eroding the Cu paper tinsel, adopt first the hydrochloric acid cleaning Graphene to clean up to guarantee iron ion; Rear employing washed with de-ionized water 10 times.Then will be transferred to the single-layer graphene of PMMA layer on the Ag nano-array, dried in 30 minutes in 50 ℃ of lower insulations, then put into acetone soln dissolving PMMA layer, and dry up through nitrogen, single-layer graphene just with two-dimentional Ag nano-array mortise, formed Ag nano-array and single-layer graphene composite substrate.
Fig. 1 is the SEM figure of the prepared Ag nano-array of present embodiment and single-layer graphene composite substrate, and Ag nano-array and single-layer graphene composite substrate are large-area ordered among the figure.Fig. 2 is the Raman spectrum picture of the prepared Ag nano-array of present embodiment and single-layer graphene composite substrate, and among the figure, the G peak position is set to 1580cm
-1, the position at 2D peak is 2700cm
-1, the position at D peak is 1350cm
-1, the ratio I of G peak and D peak intensity
G/ I
DAbout 10, prove that the prepared Graphene defective of present embodiment is few; The ratio I of 2D peak and G peak intensity
2D/ I
GAbout 3, and the 2D peak is the unimodal good symmetry that has, and proves that the prepared Graphene of present embodiment is individual layer.
Embodiment 2
Throwing on the monocrystalline silicon piece in the single face essence, is that the polystyrene nanospheres of 800 nm makes the mask plate that individual layer is closely arranged by the liquid level self-assembly method with diameter.Utilize vacuum plating unit, the Cr film of first evaporation 10 nm thickness, the Ag film of evaporation 60 nm thickness again obtain substrate on the polystyrene nanospheres mask plate.With substrate in chloroform ultrasonic 20 seconds, left standstill 10 minutes, remove the polystyrene nanospheres mask plate, and in alcohol, deionized water, clean up successively.
Adopting chemical mechanical polishing method to process thickness is the Cu paper tinsel of 25 μ m, smooth to guarantee Cu paper tinsel surface clean; Again under 1020 ℃, in methane and hydrogen mixed gas atmosphere, adopt chemical Vapor deposition process at the Cu paper tinsel of the processing single-layer graphene of growing, in the Graphene process of growth, the flow of methane and hydrogen is controlled to be respectively 35sccm and 6sccm.At the single-layer graphene surface-coated PMMA layer of growing, be cured in 30 minutes in 120 ℃ of lower insulations, then be put into ferric chloride Solution with corrosion Cu paper tinsel.
After eroding the Cu paper tinsel, adopt first the hydrochloric acid cleaning Graphene to clean up to guarantee iron ion; Rear employing washed with de-ionized water 10 times.Then will be transferred to the single-layer graphene of PMMA layer on the Ag nano-array, dried in 30 minutes in 50 ℃ of lower insulations, then put into acetone soln dissolving PMMA layer, and dry up through nitrogen, single-layer graphene just with two-dimentional Ag nano-array mortise, formed Ag nano-array and single-layer graphene composite substrate.
Fig. 3 is the SEM figure of the prepared Ag nano-array of this example and single-layer graphene composite substrate, and Ag nano-array and single-layer graphene composite substrate are large-area ordered among the figure.Fig. 4 is the Raman spectrum picture of the prepared Ag nano-array of present embodiment and single-layer graphene composite substrate, and among the figure, the G peak position is set to 1580cm
-1, the position at 2D peak is 2700cm
-1, the position at D peak is 1350cm
-1, the ratio I of G peak and D peak intensity
G/ I
DAbout 5, it is few to prove that present embodiment gets the Graphene defective; The ratio I of 2D peak and G peak intensity
2D/ I
GAbout 4, and the 2D peak is the unimodal good symmetry that has, and proves that the prepared Graphene of this example is individual layer.
The above embodiment has only expressed several embodiment of the present invention; it describes comparatively concrete and detailed; not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a noble metal nano array and single-layer graphene composite substrate is characterized in that, comprising:
Single-layer graphene layer and noble metal nano array layer.
2. noble metal nano array as claimed in claim 1 and single-layer graphene composite substrate is characterized in that:
Described noble metal nano array layer comprises Cr nanometer thin rete and noble metal nano thin film layer.
3. noble metal nano array as claimed in claim 1 and single-layer graphene composite substrate is characterized in that:
Described noble metal film is the Ag nano thin-film.
4. the preparation method of each described noble metal nano array and single-layer graphene composite substrate in the claim 1～3 is characterized in that, comprises step:
Step 1 adopts Vacuum Coating method to prepare the noble metal nano array layer;
Step 2 adopts chemical Vapor deposition process to prepare the single-layer graphene layer;
Step 3 is transferred to the single-layer graphene layer on the noble metal nano array layer, obtains noble metal nano array and single-layer graphene composite substrate.
5. the preparation method of noble metal nano array as claimed in claim 4 and single-layer graphene composite substrate is characterized in that:
Step 1 further may further comprise the steps:
1-1 adopts the liquid level self-assembly method at self-assembly substrate preparation nanometer ball mask plate;
1-2 utilizes Vacuum Coating method to plate successively Cr nano thin-film, noble metal nano film on the nanometer ball mask plate;
1-3 removes the nanometer ball mask plate, obtains the noble metal nano array.
6. the preparation method of noble metal nano array as claimed in claim 5 and single-layer graphene composite substrate is characterized in that:
Described nanometer ball mask plate is the polystyrene nanospheres mask plate, and wherein the polystyrene nanospheres diameter is 460～800nm.
7. the preparation method of noble metal nano array as claimed in claim 5 and single-layer graphene composite substrate is characterized in that:
To adopt thermal evaporation plating method successively evaporation Cr nano thin-film, noble metal nano film on the nanometer ball mask plate among the step 1-2.
8. the preparation method of noble metal nano array as claimed in claim 4 and single-layer graphene composite substrate is characterized in that:
Step 2 further may further comprise the steps:
2-1 adopts chemical mechanical polishing method to process metal base;
2-2 adopts chemical Vapor deposition process deposited monolayers Graphene on metal base;
2-3 applies glue-line at single-layer graphene;
2-4 adopts the substrate of chemical etching method corroding metal to obtain being coated with the single-layer graphene of glue-line;
And step 3 further may further comprise the steps:
The single-layer graphene that 3-1 is coated with step 2.4 gained glue-line is transferred on the noble metal nano array after cleaning, and dries;
Remove glue-line after the 3-2 oven dry, dry up through nitrogen, obtain noble metal nano array and single-layer graphene composite substrate.
9. the preparation method of noble metal nano array as claimed in claim 8 and single-layer graphene composite substrate is characterized in that:
Described metal base is the Cu paper tinsel, and described glue-line is polymethyl methacrylate layers.
10. the preparation method of noble metal nano array as claimed in claim 8 and single-layer graphene composite substrate is characterized in that:
Drying condition described in the step 3-1 is 50 ℃ of lower insulations 30 minutes.
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