CN102659098A - Equipment and method for preparing graphene - Google Patents
Equipment and method for preparing graphene Download PDFInfo
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- CN102659098A CN102659098A CN2012101578700A CN201210157870A CN102659098A CN 102659098 A CN102659098 A CN 102659098A CN 2012101578700 A CN2012101578700 A CN 2012101578700A CN 201210157870 A CN201210157870 A CN 201210157870A CN 102659098 A CN102659098 A CN 102659098A
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Abstract
The invention discloses equipment and a method for preparing graphene. The equipment mainly comprises a negative ion source, an analysis magnet, a scanning system, a sample stand, a beam integrator and a vacuum chamber. By adopting the equipment, carbon cluster ions can be injected into a substrate within a range that energy is 5-30keV; then, carbon is separated out from the surface of the substrate to form graphene through annealing treatment by utilizing the characteristic that the dissolvability of the carbon at different temperature is different in the substrate. By adopting the equipment and the method disclosed by the invention, the graphene with large area, few defects, few number of layers and evenly distributed number of layer can be prepared. The prepared graphene can be used as electrode materials of lithium ion batteries and super capacitors. A new way is provided for applying the graphene in industrial products on a large scale, such as the lithium ion batteries and the capacitors.
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 under finite temperature, freely to exist "; 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, like 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 silit 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 carbonaceousfuels such as ethanol to have in growth on the substrate of catalyst metal nanometer crystal layer to produce Graphene, and 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
To 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 Vakuumkammer, negative ion source, analyzing magnet, scanning system, specimen holder are in the Vakuumkammer, and negative ion source is used for producing group's cluster ion; Analyzing magnet is used for deflection from group's cluster ion of negative ion source, and from this cluster ion, selecting needed cluster ion, and the group's of adjusting ion beam flow to suitable size; Scanning system is used for scanning the group's cluster ion from analyzing magnet;
Described specimen holder comprises Metallic rod, isolator, sample panel, line jack and diaphragm; Metallic rod is fixedly connected with sample panel through isolator; Can promote the sample panel move left and right through Metallic rod; Sample panel connects the line totalizing instrument through 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 fixedly connected with sample panel through isolator; Can promote the sample panel move left and right through 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 through the line jack.
Above-mentioned inhibition electrode is fixedly connected with the Vakuumkammer inwall through 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, through analyzing magnet deflection from the carbon cluster ion of negative ion source, from carbon cluster ion, selecting the carbon cluster ion of required group bunch size, and regulate carbon cluster ion line to suitable size;
S3, through scanning system scanning carbon cluster ion from analyzing magnet;
S4, the hole of carbon cluster ion on diaphragm or inhibition electrode plate of scanning through 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 through the size of control diaphragm through 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
To combine accompanying drawing to further specify technical scheme of the present invention below.
Referring to Fig. 1, present device mainly comprises: negative ion source 1 is used for producing group's cluster ion; Analyzing magnet 2 is used for deflection from group's cluster ion of negative ion source 1, and from this cluster ion, selecting needed cluster ion, and the group's of adjusting ion beam flow to suitable size; Scanning system 3 is used for scanning the group's ion beam 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 group's 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 Vakuumkammer.
Negative ion source mainly comprises caesium stove, 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, and caesium steam arrives the surface with the concave type ionization device of the armouring tantalum wire coiled of big current flow heats, and 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 group's bunch negative ion spilt, that is, produce carbon cluster ion; The carbon cluster ion that produces quickens down to move to extraction electrode an extraction electrode negative voltage effect that is higher than the target current potential, is finally drawn by extraction electrode.
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 group's cluster ion through 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 in magnetic field, to have different deflection radius is selected required carbon cluster ion, regulates the magnetic field size through 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 as far as 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 through analyzing magnet smoothly through 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, through adding respectively that perpendicular to a cluster ion progressive direction, level and vertical direction the electric field of intercropping linear change at any time realizes.For example; Can be through regulating the voltage swing of horizontal scan direction; It is original 70% that the line that arrives sample panel is reduced to, the voltage swing of re-adjustment vertical sweep direction, 50% when making the line that arrives sample panel be reduced to beginning; 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, and Metallic rod 5 is passed the Vakuumkammer outer wall through vacuum adapter; The one of which end is outside Vakuumkammer; The other end is fixedly connected with sample panel 7 through isolator 6, and operator can one bring in move left and right sample panel 7 through push-and-pull Metallic rod 5 outside Vakuumkammer, to adjust the injection phase of carbon cluster ion.Sample panel 7 also connects the line totalizing instruments through line jack 8, and the line totalizing instrument is used for counting being injected on the sample panel 7 the group's 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 Vakuumkammer inwall through isolator 10, and be positioned at sample panel 7 fronts, isolator 10 will suppress electrode 9 and separate with the Vakuumkammer inwall.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, and suppressing electrode 9 can provide the voltage source of 300V voltage to be connected through voltage jack 11 with outside one, and voltage source is used for negative voltage to inhibition electrode 9 being provided; 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 through 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 through the shape and size in adjustment hole, thereby reach the purpose of control gained Graphene area; Line jack 8 is vacuum adapter with voltage jack 11, can guarantee that Vakuumkammer 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, through analyzing magnet deflection from the carbon cluster ion of negative ion source, from this carbon cluster ion, selecting the carbon cluster ion of required group bunch size, and regulate carbon cluster ion line to suitable size, preferred line size of the present invention is 0.5 ~ 5 μ A;
S3, through 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 through 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 through the carbon cluster ion after the scanning system scanning;
Adopt Ni/SiO in this practical implementation
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 vapor deposition 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 mfs 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 practical implementation 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 ℃, in this process, reduce with temperature, 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) are for regulating C respectively under 10keV, 15keV, 20keV energy condition
1-C
10The line size of group's cluster ion, resulting C
1-C
10The mass spectrum of group's cluster ion; 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
4Group's cluster ion is injected into Ni/SiO
2The Graphene that on/Si substrate, after annealing, obtains, 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
1Group's cluster ion is injected into Ni/SiO
2The Graphene that on/Si substrate, after annealing, obtains, 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 vapor deposition 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, result such as Fig. 4 and shown in 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 ionic group bunch size increase 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 group's 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 basically, 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 (10)
1. an equipment for preparing Graphene is characterized in that, comprising:
Negative ion source, analyzing magnet, scanning system, specimen holder, line totalizing instrument and Vakuumkammer, negative ion source, analyzing magnet, scanning system, specimen holder are in the Vakuumkammer, and negative ion source is used for producing group's cluster ion; Analyzing magnet is used for deflection from group's cluster ion of negative ion source, and from this cluster ion, selecting needed cluster ion, and the group's of adjusting ion beam flow to suitable size; Scanning system is used for scanning the group's cluster ion from analyzing magnet; Described specimen holder comprises Metallic rod, isolator, sample panel, line jack and diaphragm; Metallic rod is fixedly connected with sample panel through isolator; Can promote the sample panel move left and right through Metallic rod; Sample panel connects the line totalizing instrument through the line jack, and diaphragm is between sample panel and scanning system and face sample panel.
2. the equipment of preparation Graphene according to claim 1 is characterized in that:
Described specimen holder can also for:
Specimen holder comprises Metallic rod, isolator, sample panel, line jack, suppresses electrode and voltage jack; Metallic rod is fixedly connected with sample panel through isolator; Can promote the sample panel move left and right through 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 through the line jack.
3. the equipment of preparation Graphene according to claim 2 is characterized in that:
Described inhibition electrode is fixedly connected with the Vakuumkammer inwall through isolator.
4. the equipment of preparation Graphene according to claim 2 is characterized in that:
The metal sheet that constitutes described inhibition electrode is aluminium sheet or stainless steel plate.
5. the equipment of preparation Graphene according to claim 2 is characterized in that:
The hole of described inhibition electrode bottom surface is a square hole, and the hole is of a size of 10x10 mm
2
6. the equipment of preparation Graphene according to claim 2 is characterized in that:
Described inhibition electrode is a trapezoidal concave surface.
7. adopt each described equipment among the claim 1-6 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, through analyzing magnet deflection from the carbon cluster ion of negative ion source, from carbon cluster ion, selecting the carbon cluster ion of required group bunch size, and regulate carbon cluster ion line to suitable size;
S3, through scanning system scanning carbon cluster ion from analyzing magnet;
S4, the hole of carbon cluster ion on diaphragm or inhibition electrode plate of scanning through 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.
8. the method for preparing Graphene according to claim 7 is characterized in that:
Described substrate is Ni/SiO
2/ Si, single crystal Cu, polycrystalline copper, monocrystalline nickel or polycrystalline nickel.
9. the method for preparing Graphene according to claim 8 is characterized in that:
Described Ni/SiO
2Ni film thickness 50nm in the/Si substrate, SiO
2Thickness is 300nm.
10. the method for preparing Graphene according to claim 7 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103266306A (en) * | 2013-05-22 | 2013-08-28 | 宜昌后皇真空科技有限公司 | Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique |
| 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 |
| CN103928282A (en) * | 2014-05-06 | 2014-07-16 | 武汉大学 | Ion injection sample platform |
| CN104736477A (en) * | 2012-10-15 | 2015-06-24 | 信越化学工业株式会社 | Method for producing nanocarbon film and nanocarbon film |
| CN108358189A (en) * | 2018-01-03 | 2018-08-03 | 中国科学院电工研究所 | A method of 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 | Two-dimensional material doping method based on cluster ion implantation |
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| CN102373433A (en) * | 2011-11-21 | 2012-03-14 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
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Patent Citations (2)
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| EP1452485A2 (en) * | 2003-02-27 | 2004-09-01 | Fuji Xerox Co., Ltd | Manufacturing apparatus and method for carbon nanotube |
| CN102373433A (en) * | 2011-11-21 | 2012-03-14 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104736477A (en) * | 2012-10-15 | 2015-06-24 | 信越化学工业株式会社 | Method for producing nanocarbon film and nanocarbon film |
| CN104736477B (en) * | 2012-10-15 | 2016-11-02 | 信越化学工业株式会社 | The manufacture method of nano-carbon film and nano-carbon film |
| CN103266306A (en) * | 2013-05-22 | 2013-08-28 | 宜昌后皇真空科技有限公司 | Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique |
| 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 |
| CN103928282A (en) * | 2014-05-06 | 2014-07-16 | 武汉大学 | Ion injection sample platform |
| CN108358189A (en) * | 2018-01-03 | 2018-08-03 | 中国科学院电工研究所 | A method of 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 | Two-dimensional material doping method based on cluster ion implantation |
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