CN102659098B - Equipment and method for preparing graphene - Google Patents
Equipment and method for preparing graphene Download PDFInfo
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- CN102659098B CN102659098B CN2012101578700A CN201210157870A CN102659098B CN 102659098 B CN102659098 B CN 102659098B CN 2012101578700 A CN2012101578700 A CN 2012101578700A CN 201210157870 A CN201210157870 A CN 201210157870A CN 102659098 B CN102659098 B CN 102659098B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 61
- 239000000758 substrate Substances 0.000 claims abstract description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 36
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 230000005764 inhibitory process Effects 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000005477 sputtering target Methods 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000010884 ion-beam technique Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 77
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 150000001450 anions Chemical class 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 239000007943 implant Substances 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 42
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910052792 caesium Inorganic materials 0.000 description 6
- 230000002950 deficient Effects 0.000 description 6
- 150000001721 carbon Chemical group 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 230000033001 locomotion Effects 0.000 description 4
- 238000001819 mass spectrum Methods 0.000 description 4
- 238000010297 mechanical methods and process Methods 0.000 description 4
- 230000005226 mechanical processes and functions Effects 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000002513 implantation Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 208000031968 Cadaver Diseases 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 230000035924 thermogenesis Effects 0.000 description 1
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Abstract
本发明公开了一种制备石墨烯的设备及方法，该设备主要包括负离子源、分析磁铁、扫描系统、样品架、束流积分仪和真空室，采用上述设备能在能量为5-30keV的范围内进行碳团簇离子在衬底中的注入，然后利用不同温度下碳在衬底中溶解度的不同，经退火处理，使碳从衬底表面析出形成石墨烯。采用本发明设备和方法可以制备面积大、缺陷少、层数少且层数分布均匀的石墨烯，所制备的石墨烯可用作锂离子电池、超级电容器的电极材料，为石墨烯在锂电池、电容器等工业化产品中的大规模应用提供了一种新的途径。
The invention discloses a device and method for preparing graphene. The device mainly includes an anion source, an analysis magnet, a scanning system, a sample holder, a beam integrator and a vacuum chamber. The device can be used in the energy range of 5-30keV Implant carbon cluster ions into the substrate, and then use the difference in solubility of carbon in the substrate at different temperatures to anneal to precipitate carbon from the surface of the substrate to form graphene. The equipment and method of the present invention can be used to prepare graphene with large area, few defects, few layers and uniform distribution of layers. The prepared graphene can be used as electrode materials for lithium ion batteries and supercapacitors. Large-scale applications in industrialized products such as , capacitors, etc. provide a new way.
Description
Technical field
The invention belongs to ionic fluid and technical field of material, relate in particular to a kind of equipment and method for preparing Graphene.
Background technology
2004, the Andre Geim research group of Univ Manchester UK prepares stable Graphene first, broken through the one theory of classical " the thermodynamics fluctuation does not allow two dimensional crystal freely to exist " under finite temperature, cause the very big shock of whole physics and material educational circles, caused the research boom of Graphene thus.The ideal graphene-structured can be regarded as monoatomic layer graphite, is by sp
2The class six-ring benzene unit that the hydridization carbon atom forms and the two dimensional crystal material of infinite expanding also are the thinnest in the world present material-monatomic thickness of material.Graphene not only has excellent electric property, outstanding heat conductivility and extraordinary specific surface area, but also has some particular performances, as perfect quantum tunneling effect, half-integer quantum hall effect, a series of character such as specific conductivity of never disappearing.Have so numerous peculiar character just because of grapheme material, caused different field scientists' such as physics, chemistry, material very big research interest, also made Graphene have great application prospect in fields such as electronics, information, the energy, material and biological medicines.
At present, preparation method of graphene mainly contains mechanical process and chemical method two big classes.Mechanical process comprises micromechanics partition method, epitaxy method and heating silicon carbide method, and chemical method comprises chemical reduction method and chemical cleavage method etc.No matter be to adopt mechanical process or chemical preparation Graphene, all there is the unmanageable problem of size (area and thickness).Before the present invention, China was in publication application on May 25 " a kind of preparation method of graphene " in 2011, application number is 201110057535.9, the method of this application is to utilize the flame of carbonaceous fuels such as ethanol to have in growth on the substrate of catalyst metal nanometer crystal layer to produce Graphene, this method is simple to operate, but adopts this method to be difficult to guarantee the homogeneity and the continuity of prepared Graphene.
Summary of the invention
At the deficiency that prior art exists, the present invention proposes a kind of mechanical process and chemical method and accurate Apparatus and method for of the preparation Graphene of controlling dimension of differing from.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
One, a kind of equipment for preparing Graphene comprises:
Negative ion source, analyzing magnet, scanning system, specimen holder, line totalizing instrument and vacuum chamber, negative ion source, analyzing magnet, scanning system, specimen holder are in the vacuum chamber, and negative ion source is used for producing the cluster ion; Analyzing magnet is used for deflection from the cluster ion of negative ion source, selecting needed cluster ion from this cluster ion, and regulates the cluster ion beam current to suitable size; Scanning system is used for scanning the cluster ion from analyzing magnet;
Described specimen holder comprises metallic rod, isolator, sample panel, line jack and diaphragm, metallic rod is fixedlyed connected with sample panel by isolator, can promote the sample panel move left and right by metallic rod, sample panel connects the line totalizing instrument by the line jack, and diaphragm is between sample panel and scanning system and face sample panel.
Above-mentioned specimen holder also has following preferred version:
Specimen holder comprises metallic rod, isolator, sample panel, line jack, suppresses electrode and voltage jack, metallic rod is fixedlyed connected with sample panel by isolator, can promote the sample panel move left and right by metallic rod, suppressing electrode is the concave surface that is surrounded by metal base plate with holes and two relative metal sheets, its between sample panel and scanning system and its opening the sample panel front is encased, suppress electrode and be connected with the voltage jack, sample panel connects the line totalizing instrument by the line jack.
Above-mentioned inhibition electrode is fixedlyed connected with the vacuum chamber inwall by isolator.
The metal sheet that above-mentioned formation suppresses electrode is aluminium sheet or stainless steel plate.
The hole of above-mentioned inhibition electrode bottom surface is a square hole, and the hole is of a size of 10x10 mm
2
Above-mentioned inhibition electrode is a trapezoidal concave surface.
Two, adopt aforesaid device to prepare the method for Graphene, comprise step:
S1, be sputtering target, utilize above-mentioned negative ion source to produce carbon cluster ion with the high-density graphite rod;
S2, by analyzing magnet deflection from the carbon cluster ion of negative ion source, from carbon cluster ion, selecting the carbon cluster ion of required cluster size, and regulate the carbon cluster ion line to suitable size;
S3, by scanning system scanning carbon cluster ion from analyzing magnet;
S4, the hole of carbon cluster ion on diaphragm or inhibition electrode plate of scanning by scanning system are injected on the substrate that places on the sample panel;
S5, take off the substrate that injects carbon cluster ion, it is carried out anneal, promptly on substrate, obtain Graphene.
Above-mentioned substrate is Ni/SiO
2/ Si, single crystal Cu, polycrystalline copper, monocrystalline nickel or polycrystalline nickel.
As preferably, Ni/SiO
2Ni film thickness 50nm in the/Si substrate, SiO
2Thickness is 300nm.
The selection process of above-mentioned anneal is: 900 ℃ keep 50 minutes after, make temperature reduce to 725 ℃ with the speed of 5-20 ℃/min from 900 ℃.The purpose of the substrate that injects carbon cluster ion being carried out anneal is: utilize that carbon makes the carbon that is injected in the metal substrate separate out the formation Graphene from the surface in the difference of metal substrate solubleness under the differing temps.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1, prepared graphene impurity of the present invention is few, and defective is few, the number of plies is few, area is big, productive rate is high, is fit to suitability for industrialized production;
2, adopt the present invention accurately to control, control the thickness of Graphene, control the area of Graphene by the size of control diaphragm by controlling implantation dosage to the size of prepared Graphene;
3, the multi-layer graphene prepared of the inventive method can be used as the electrode materials of lithium ion battery, ultracapacitor, for the large-scale application of Graphene in industrialization products such as lithium cell, electrical condenser provides a kind of new approach.
Description of drawings
Fig. 1 is the schematic top plan view of present device, wherein, and 1-negative ion source, 2-analyzing magnet, 3-scanning system, 4-specimen holder;
Fig. 2 is the structural representation of a kind of embodiment of specimen holder of the present invention, wherein, the 5-metallic rod, the 6-isolator, the 7-sample panel, 8-line jack, 9-suppress electrode, 10-isolator, 11-voltage jack, 12-hole;
Fig. 3 is the mass spectrum of the carbon cluster ion that present device produced;
Fig. 4 is the Raman spectrogram of the prepared Graphene of the present invention;
Fig. 5 is the Raman spectrogram of the prepared Graphene of the present invention.
Embodiment
Further specify technical scheme of the present invention below in conjunction with accompanying drawing.
Referring to Fig. 1, present device mainly comprises: negative ion source 1 is used for producing the cluster ion; Analyzing magnet 2 is used for deflection from the cluster ion of negative ion source 1, selecting needed cluster ion from this cluster ion, and regulates the cluster ion beam current to suitable size; Scanning system 3 is used for scanning the cluster ionic fluid from analyzing magnet 2, makes the repeatedly even inswept surface that places the substrate on the sample panel of ionic fluid, with the homogeneity that guarantees to inject; Specimen holder 4 be used for receiving the cluster ion from scanning system 3, and diplomatic corps's cluster ion is injected in the substrate that is placed on the sample panel.Above-mentioned negative ion source 1, analyzing magnet 2, scanning system 3, specimen holder 4 all are positioned at a vacuum chamber.
Negative ion source mainly comprises the caesium stove, the ionization device, sputtering target (being specially the carbon sputtering target) and extraction electrode, its principle of work is: the liquid metal caesium in the caesium stove is through adding thermogenesis caesium steam, caesium steam arrives the surface with the concave type ionization device of the armouring tantalum wire coiled of big current flow heats, cold caesium gas molecule runs into hot tantalum wire and ionization, the cesium ion that produces under negative target voltage effect accelerated motion to sputtering target, the form of carbon atom in the sputtering target with the cluster negative ion spilt, promptly, produce carbon cluster ion, the carbon cluster ion that produces quickens finally to be drawn by extraction electrode to the extraction electrode motion under an extraction electrode negative voltage effect that is higher than the target current potential.
The carbon cluster ion that produces when negative ion source moves to analyzing magnet, analyzing magnet carries out deflection to carbon cluster ion, can select required cluster ion by the outward current of regulating analyzing magnet in advance, and the carbon cluster ion line transferred to suitable size, the preferred line size of the present invention is 0.5 ~ 5 μ A.Analyzing magnet is that the principle of utilizing the ion of different specific charges to have different deflection radius in magnetic field is selected required carbon cluster ion, regulates the magnetic field size by the size of current that changes analyzing magnet, selects required cluster ion thereby reach.For the purpose of the present invention, each negative ion source all can produce various carbon cluster ion, under identical probe voltage and magneticstrength, different carbon cluster ions has different movement paths, but for carbon cluster ion of the same race, change the movement path that probe voltage or magneticstrength all can change carbon cluster ion, therefore, can make needed a kind of carbon cluster ion arrive scanning system by analyzing magnet smoothly by the probe voltage of negative ion source and the magneticstrength of analyzing magnet are regulated.
Scanning system is the homogeneity when guaranteeing that the carbon cluster ion big area is injected substrate, by adding respectively that perpendicular to cluster ion progressive direction, level and vertical direction the electric field of intercropping linear change at any time realizes.For example, can be by regulating the voltage swing of horizontal scan direction, make the line that arrives sample panel be reduced to original 70%, the voltage swing of re-adjustment vertical sweep direction, when making the line that arrives sample panel be reduced to beginning 50%, 50% line of losing is the part on the nonlinear bundle spot of track while scan border, can obtain scanning uniform high-quality carbon cluster ion bundle at last.
Fig. 2 is a kind of embodiment of specimen holder 4 of the present invention, as shown in the figure, specimen holder 4 comprises metallic rod 5, isolator 6, sample panel 7, line jack 8, suppresses electrode 9, isolator 10, voltage jack 11, metallic rod 5 is passed the vacuum chamber outer wall by vacuum adapter, the one end is outside vacuum chamber, the other end is fixedlyed connected with sample panel 7 by isolator 6, and operator can one bring in move left and right sample panel 7 by push-and-pull metallic rod 5 outside vacuum chamber, with the injection phase of adjustment carbon cluster ion.Sample panel 7 also connects the line totalizing instruments by line jack 8, and the line totalizing instrument is used for counting being injected on the sample panel 7 the cluster ion in the substrate, and judging whether to inject required dosage, thereby decision is to continue to inject, and still stops to inject.Isolator 6 separates metallic rod 5 and sample panel 7, is the accuracy in order to count.
Suppress electrode 9 and be fixed in the vacuum chamber inwall by isolator 10, and be positioned at sample panel 7 fronts, isolator 10 will suppress electrode 9 and the vacuum chamber inwall separates.Suppress electrode 9 and be the trapezoidal concave surface that surrounded by with holes 12 aluminum soleplate and two relative up and down aluminium sheets, wherein, the outside of aluminum soleplate (being the upper surface that suppresses electrode 9 among Fig. 2) is towards scanning system, the opening that suppresses electrode 9 surrounds towards the sample panel that is positioned at its rear and with the front of sample panel, suppressing electrode 9 can provide the voltage source of 300V voltage to be connected by voltage jack 11 with one of outside, and voltage source is used for providing negative voltage to suppressing electrode 9; Hole on the metal base plate of inhibition electrode 9 is a square hole, and it is of a size of 10x10mm
2The inhibition electrode 9 that connects behind the negative voltage can stop most secondary electron, carbon cluster ion from scanning system arrives sample panel 7 by the hole 12 that suppresses on electrode 9 metal base plates, the effect of diaphragm is played in this hole 12, can control bundle shape of spot and the size on the substrate on the sample panel by the shape and size of adjusting the hole, thereby reach the purpose of control gained Graphene area; Line jack 8 and voltage jack 11 are vacuum adapter, can guarantee that vacuum chamber is air tight.
Correspondingly, the method for utilizing aforesaid device to prepare Graphene may further comprise the steps:
S1, be sputtering target, utilize above-mentioned negative ion source to produce carbon cluster ion with the high-density graphite rod
Negative ion source among the present invention can provide the energy of 5～30keV scope.
S2, by analyzing magnet deflection from the carbon cluster ion of negative ion source, from this carbon cluster ion, selecting the carbon cluster ion of required cluster size, and regulate the carbon cluster ion line to suitable size, preferred line size of the present invention is 0.5 ~ 5 μ A;
S3, by scanning system scanning carbon cluster ion bundle from analyzing magnet, make the carbon cluster ion after scanning can evenly be injected into the substrate that places on the sample panel;
Scanning system among the present invention can provide the 0-1000V sweep voltage, can control the scanning area of carbon cluster ion by the voltage swing of adjusting level respectively and vertical sweep direction, the carbon cluster ion after the scanning can evenly be injected in the substrate that is placed on the sample panel.
S4, be injected into the substrate that places on the sample panel through diaphragm or the hole that suppresses on the electrode plate by the carbon cluster ion after the scanning system scanning;
Adopt Ni/SiO in this concrete enforcement
2/ Si substrate, carbon cluster ion injects the Ni film, and this substrate adopts following method to obtain:
The SiO that utilizes thermal evaporation techniques cleaning
2The thick nickel film of evaporation one deck 50nm obtains Ni/SiO on the/Si wafer
2/ Si substrate, wherein, SiO
2SiO on the/Si wafer
2Layer thickness is 300nm.
In addition, substrate also can adopt metallic films such as single crystal Cu, polycrystalline copper, monocrystalline nickel or polycrystalline nickel.
S5, take off the substrate that injects carbon cluster ion, it is carried out anneal, promptly on substrate layer, obtain Graphene.
The substrate that has injected carbon cluster ion is put into vacuum annealing furnace carry out thermal anneal process, the annealing process that is adopted in this concrete enforcement is: kept 50 minutes at 900 ℃, carbon is spread in the metallic nickel film of substrate, then, with the speed of 5-20 ℃/min temperature is dropped to 725 ℃ from 900 ℃, reduce with temperature in this process, the solubleness of carbon in the nickel film also decreases, carbon is separated out from nickel film surface, thereby forms Graphene on nickel film surface.
Referring to Fig. 3, Fig. 3 (a), 3(b), 3(c) under 10keV, 15keV, 20keV energy condition, regulating C respectively
1-C
10Cluster ionic line size, resulting C
1-C
10Cluster ionic mass spectrum, line totalizing instrument in The data aforesaid device of this mass spectrum measures, this mass spectrum can prove that present device is the carbon cluster ion that can provide different, and the line that obtains is suitable, can satisfy the preparation demand needs of Graphene.
Adopt 3 groups of Graphene samples of method for preparing a-c, the area of these 3 groups of samples is 10x10mm
2, sample a and b all are under the 20keV energy condition, select C respectively
2And C
4Cluster is ion implantation to Ni/SiO
2The Graphene that obtains on/Si the substrate, after annealing, implantation dosage is 8x10
15Atoms/cm
2, the injection energy of single carbon atom is respectively 10keV and 5keV among sample a and the b; Sample c is under the 10keV energy condition, selects C
1Cluster is ion implantation to Ni/SiO
2The Graphene that obtains on/Si the substrate, after annealing, implantation dosage is 8x10
15Atoms/cm
2, the injection energy of its single carbon atom is 10keV.Above-mentioned Ni/SiO
2/ Si substrate all adopts following method to obtain: the SiO that utilizes thermal evaporation techniques cleaning
2The thick nickel film of evaporation one deck 50nm obtains Ni/SiO on the/Si wafer
2/ Si substrate, wherein, SiO
2SiO on the/Si wafer
2Layer thickness is 300nm.
Sample a, b and c are carried out Raman spectrum characterize, the result as shown in Figure 4 and Figure 5, among Fig. 4,1353 cm
-1The D peak at place is the defective peak, the randomness of reaction Graphene; 1581cm
-1The G peak at place is the characteristic peak of carbon sp2 structure, the symmetry and the crystallization degree of reaction Graphene, 2705～2712 cm
-1The 2D peak at place comes from the inelastical scattering of two biphonons.I
D/ I
GBe worth more little, represent in the Graphene defective more less, I
2D/ I
GAnd the position at 2D peak and halfwidth represent the number of plies of Graphene, wherein, and I
D, I
G, I
2DThe intensity of representing D peak in the above-mentioned Raman spectrogram, G peak, 2D peak respectively.As can be seen from Figure 4, the about layer 2-3 graphite of sample a and b, and defective is less, and reduce with increase of ion cluster size and injection energy, the defective of the Graphene that forms has minimizing trend, but the 2D peak position moves to right, so the number of plies does not reduce.Therefore the formation that whether helps Graphene of big cluster ion does not also obtain proof.As can be seen from Figure 5, the number of plies of sample a and c is equal substantially, but the defective of sample a significantly reduces, and therefore under identical energy condition, big carbon cluster ion more helps the formation of better quality Graphene.
Claims (9)
1. an equipment for preparing Graphene is characterized in that, comprising:
Negative ion source, analyzing magnet, scanning system, specimen holder, line totalizing instrument and vacuum chamber, negative ion source, analyzing magnet, scanning system, specimen holder are in the vacuum chamber, and negative ion source is used for producing the cluster ion; Analyzing magnet is used for deflection from the cluster ion of negative ion source, selecting needed cluster ion from this cluster ion, and regulates the cluster ion beam current to suitable size; Scanning system is used for scanning the cluster ion from analyzing magnet; Described specimen holder comprises metallic rod, isolator, sample panel, line jack, suppresses electrode and voltage jack, metallic rod is fixedlyed connected with sample panel by isolator, can promote the sample panel move left and right by metallic rod, suppressing electrode is the concave surface that is surrounded by metal base plate with holes and two relative metal sheets, its between sample panel and scanning system and its opening the sample panel front is encased, suppress electrode and be connected with the voltage jack, sample panel connects the line totalizing instrument by the line jack.
2. the equipment of preparation Graphene according to claim 1 is characterized in that:
Described inhibition electrode is fixedlyed connected with the vacuum chamber inwall by isolator.
3. the equipment of preparation Graphene according to claim 1 is characterized in that:
The metal sheet that constitutes described inhibition electrode is aluminium sheet or stainless steel plate.
4. the equipment of preparation Graphene according to claim 1 is characterized in that:
The hole of described inhibition electrode bottom surface is a square hole, and the hole is of a size of 10x10mm
2
5. the equipment of preparation Graphene according to claim 1 is characterized in that:
Described inhibition electrode is a trapezoidal concave surface.
6. adopt each described equipment among the claim 1-5 to prepare the method for Graphene, it is characterized in that, comprise step:
S1, be sputtering target, utilize above-mentioned negative ion source to produce carbon cluster ion with the high-density graphite rod;
S2, by analyzing magnet deflection from the carbon cluster ion of negative ion source, from carbon cluster ion, selecting the carbon cluster ion of required cluster size, and regulate the carbon cluster ion line to suitable size;
S3, by scanning system scanning carbon cluster ion from analyzing magnet;
S4, the hole of carbon cluster ion on diaphragm or inhibition electrode plate of scanning by scanning system are injected into the substrate that places on the sample panel;
S5, take off the substrate that injects carbon cluster ion, it is carried out anneal, promptly on substrate, obtain Graphene.
7. the method for preparing Graphene according to claim 6 is characterized in that:
Described substrate is Ni/SiO
2/ Si, single crystal Cu, polycrystalline copper, monocrystalline nickel or polycrystalline nickel.
8. the method for preparing Graphene according to claim 7 is characterized in that:
Described Ni/SiO
2Ni film thickness 50nm in the/Si substrate, SiO
2Thickness is 300nm.
9. the method for preparing Graphene according to claim 6 is characterized in that:
Described annealing treating process is: 900 ℃ keep 50 minutes after, make temperature reduce to 725 ℃ with the speed of 5-20 ℃/min from 900 ℃.
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| KR102115631B1 (en) * | 2012-10-15 | 2020-05-26 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Method for producing nanocarbon film and nanocarbon film |
| CN103266306B (en) * | 2013-05-22 | 2015-11-18 | 宜昌后皇真空科技有限公司 | A kind of PVD technology prepares the method for Graphene or ultrathin carbon films |
| CN103695869A (en) * | 2013-12-20 | 2014-04-02 | 上海中电振华晶体技术有限公司 | Preparation method of graphene film |
| CN103928282B (en) * | 2014-05-06 | 2016-03-16 | 武汉大学 | A kind of ion implantation sample stage |
| CN108358189B (en) * | 2018-01-03 | 2020-06-16 | 中国科学院电工研究所 | A kind of method for preparing graphene |
| CN117116772A (en) * | 2023-10-19 | 2023-11-24 | 江苏集创原子团簇科技研究院有限公司 | A two-dimensional material doping method based on cluster ion implantation |
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| CN102373433B (en) * | 2011-11-21 | 2013-02-13 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
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