CN102120574A - Method for preparing large-scale two-dimensional nanomaterial graphite - Google Patents
Method for preparing large-scale two-dimensional nanomaterial graphite Download PDFInfo
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- CN102120574A CN102120574A CN 201110060953 CN201110060953A CN102120574A CN 102120574 A CN102120574 A CN 102120574A CN 201110060953 CN201110060953 CN 201110060953 CN 201110060953 A CN201110060953 A CN 201110060953A CN 102120574 A CN102120574 A CN 102120574A
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Abstract
The invention relates to a method for preparing a large-scale two-dimensional nanomaterial graphite, comprising the following steps of: plating a nickel film with the thickness of 100-300nm on the surface of monocrystal silicon, and then injecting carbon element into the nickel film by adopting an ion implantation mode; annealing for 15min-1h at a high temperature between 600 DEG C and 1,000 DEG C and a vacuum degree of from (10-5)Pa to 1Pa, and cooling to room temperature so that carbon atoms are separated out from the nickel film and recombined. Therefore, a layer of graphite film (the film thickness depends on various experiment parameters, such as carbon injection content, and the like) can be formed on the surface of the nickel film. When a sample is put into a FeCl3 solution, the nickel film can be corroded, and the graphite film can be separated out and floats on the surface of the liquid; and at the moment, the graphite film can be transferred away from the liquid with any substrate. Therefore, the large-scale graphite film with the size of several centimeters can be prepared.
Description
Technical field
The present invention relates to a kind of two-dimensional nano material preparation method of graphene, and preparation technology, particularly a kind of mode of utilizing carbon to inject prepares the method for Graphene on a large scale, and preparation technology.The invention belongs to the material technology field.
Background technology
Graphene (graphene) is the two dimensional crystal that is made of carbon atom, and also the someone uses " mono-layer graphite " as its address.In Graphene, carbon atom is with sp
2Hydridization also is arranged in cellular hexaplanar structure.Graphene also is the basic comprising unit of other carbon material allotropic substance.
Graphene is at first to be found that by the scientist of Univ Manchester UK the discoverer of Graphene has obtained Nobel Prize in physics in 2010 by 2004.The room temperature mobility of current carrier in the Graphene〉20000 cm
2/ Vs, all higher than any semiconductor material known today, comprise the silicon materials of large-scale application in the semicon industry, be considered to the replacer of silicon in the following nano electron device.Graphene is also very extensive in the application of photoelectric field, comprises the solar cell based on Graphene, photodetector etc.Graphene all is based in the application in photoelectricity, biology and other material fields on the basis of the graphene film of growth on a large scale.
The method for preparing at present graphene film roughly has following several: tape stripping method, silicon carbide epitaxial growth method, graphite oxide reduction method, solution are directly peeled off method, chemical Vapor deposition process etc.Above-mentioned method respectively has its pros and cons: the tape stripping method can prepare high-quality Graphene, but the Graphene area of this method preparation at present can only be used for Basic Experiment Study less than 1 millimeter * 1 millimeter.Epitaxially grown Graphene on the silicon carbide, though area is big and evenly, the Graphene quality that this method obtains is still waiting to improve, and stronger interaction is arranged between Graphene and silicon carbide substrates, silicon carbide substrates is also extremely expensive.Graphite oxide reduction method or solution are directly peeled off method, though can obtain the larger area graphene film, but because preparation process has been introduced more defective in Graphene, and monolithic Graphene undersized (about 100 nanometers), thereby cause the film that obtains discontinuous, its electroconductibility is also suddenly waited to improve.Recently, investigators find to utilize chemical Vapor deposition process can prepare large-area graphene film at transiting metal surfaces such as nickel or copper, and quality is also good.But the controllability of the graphene film thickness that this method obtains is relatively poor, can grow multilayer film in uneven thickness on the nickel metal, and can only grow single thin film and a spot of bilayer film on the copper.
Summary of the invention
Technical problem:Technical problem to be solved by this invention is to propose a kind of preparation method of two-dimensional nano material Graphene on a large scale, and the mode of utilizing carbon to inject prepares graphene film, to overcome the drawback of existing all multi-methods, as the Graphene chi
Very little little, of low quality, controllable thickness is relatively poor etc.
Technical scheme:The mode that the present invention utilizes the carbon high speed ion to inject provides carbon source, prepare graphene film on a large scale: at first, at monocrystalline silicon surface plating 100-300nm nickel film, utilize ion implantation mode then, carbon is injected in the nickel film, (scald fiery temperature in order to remove hairs between 600-1000 degree centigrade, vacuum tightness 10 through taking off fire again
-5To 1 handkerchief, scald 15 minutes to the 1 hour time of fire in order to remove hairs), reduce to room temperature then, make the carbon atom generation graphene film of from the nickel film, separating out and recombinate.At last, utilize ferric chloride Solution corrosion nickel film, with any substrate this graphene film is migrated out from fluid surface then, so large-scale graphene film just completes, and big I reaches several centimetres.
This preparation technology's flow process and control condition are specific as follows:
One, nickel film preparation: adopt sputtering method (Sputtering) or pulsed laser deposition methods such as (Pulsed Laser Deposition) at monocrystalline silicon surface nickel plating film, film thickness between 100-300nm,
Two, carbon atom injects: the method for utilizing high speed ion to inject, carbon is injected into the surface of nickel film, and ion implantation dosage (Dose) is 5x10
15-5x10
16Cm
-2, energy is 500-1000eV,
Three, high temperature is scalded fire in order to remove hairs: scald fire in order to remove hairs under 600-1000 degree centigrade, scalding the fire time in order to remove hairs is 15 minutes-60 minutes, and vacuum condition is 10
-5Pa to 1Pa,
Four, nickel thin film corrosive: utilize concentration to be the ferric chloride Solution of 0.25-1 mol corrosion nickel film, make graphene film from substrate separation and swim in solution surface, etching time is 3-24 hour,
Five, graphene film shifts: the graphene film that will swim in solution surface with any substrate migrates out, and promptly obtains large-scale graphene film.
Beneficial effect:The graphene film that this method obtains has large size (several centimetres or bigger), quality is good and the adjustable advantages such as (regulating and control by the carbon implantation dosage) of thickness: compare and the tape stripping method, the Graphene size that this method obtains is very big; Than the graphite oxide reduction method, the Graphene monolithic size that this method obtains is big, and quality is higher; Than the silicon carbide epitaxial growth method, the Graphene that this method obtains is with low cost, and does not have interaction with substrate; Compare and chemical Vapor deposition process, the Graphene that this method obtains has the adjustable characteristics of thickness.And this growth method and present semiconductor technological condition bonded are very good, and wherein nickel depositing of thin film, carbon are ion implantation, to scald means such as fire in order to remove hairs all be very sophisticated technology at semicon industry at present.This has just saved exploitation and equipment cost greatly.So this growth method can promote the widespread use of Graphene in semi-conductor industry circle quickly, and can produce huge economic benefits.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is the Raman spectrogram of the graphene film of acquisition in the example 1 of the present invention.
Embodiment
The preparation method: (1) at first plates the nickel film of 100-300nm at monocrystalline silicon surface.Available sputtering method (Sputtering) or other film growth methods,
(2) utilize ion implantation mode, carbon is injected in the nickel film.The distribution available software of carbon atom in the nickel film accurately simulation draws, and the content of carbon atom also can accurately be controlled,
(3) reduce to room temperature after sample is taken off fire at a high speed, scald in order to remove hairs fiery temperature 600-1000 degree centigrade (
oC) between, vacuum tightness 10
-5Pa to 1Pa scalds 15 minutes to the one hour time of fire in order to remove hairs.So far, the nickel film surface has one deck graphene film,
(4) sample that will contain graphene film is put into ferric chloride Solution (time is more than 3 hours).The nickel film can be corroded, and graphene film can and swim in fluid surface from substrate separation,
(5) at this moment, can this film be shifted from liquid with any substrate and (can 300nm SiO be arranged with the surface
2The monocrystalline substrate of film).So large-scale graphene film promptly completes, and big I reaches several centimetres.
With reference to experiment flow shown in Figure 1, below with 3 embodiment, in allowed band, select three groups of different experiment controlled variable, implement to specify.
Embodiment 1: implement by following five steps
One, nickel film preparation: utilize sputtering method (Sputtering) to plate uniform nickel film on monocrystalline silicon piece (0.7 mm thick) surface, thickness is 300nm,
Two, carbon injects: utilize ion implantation mode that carbon is injected into the nickel film.Ion implantation energy is 600eV, and dosage is 5x10
15Cm
-2,
Three, high temperature is scalded fire in order to remove hairs: will inject sample behind the carbon and put into High Temperature Furnaces Heating Apparatus and take off fire, taking off fiery temperature is 900
oC, taking off the fire time is 30 minutes, vacuum tightness 10
-5Pa.And after taking off fire, reduce to room temperature.So far, the nickel film surface can grow one deck graphene film,
Four, nickel thin film corrosive: have the substrate of graphene film to put into ferric chloride Solution on the surface and corrode, strength of solution is 1 mol, and etching time is 10 hours.So far, the nickel film can be corroded fully, and graphene film then can separate and swim in solution surface,
Five, graphene film shifts: with the surface 300nm SiO is arranged
2The silicon substrate of film migrates out the graphene film that swims in solution surface, promptly obtains large-scale graphene film.
Obtain the Raman spectrogram of graphene film in accompanying drawing 2 by above-mentioned experimental procedure.
Embodiment 2: one, nickel film preparation: utilize sputtering method (Sputtering) to plate uniform nickel film on monocrystalline silicon piece (0.7 mm thick) surface, thickness is 300nm,
Two, carbon injects: utilize ion implantation mode that carbon is injected into the nickel film.Ion implantation energy is 1000 eV, and metering is 10
16Cm
-2,
Three, high temperature is scalded fire in order to remove hairs: will inject sample behind the carbon and put into High Temperature Furnaces Heating Apparatus and take off fire, taking off fiery temperature is 800
oC, taking off the fire time is 45 minutes, vacuum tightness 1Pa.And after taking off fire, reduce to room temperature.So far, the nickel film surface can grow one deck graphene film,
Four, nickel thin film corrosive: have the substrate of graphene film to put into ferric chloride Solution on the surface and corrode, strength of solution is 1 mol, and etching time is 10 hours.So far, the nickel film can be corroded fully, and graphene film then can separate and swim in solution surface,
Five, graphene film shifts: with the surface 300nm SiO is arranged
2The silicon substrate of film migrates out the graphene film that swims in solution surface, promptly obtains large-scale graphene film.
Omit detected result.Embodiment 3:
One, nickel film preparation: utilize sputtering method (Sputtering) to plate uniform nickel film on monocrystalline silicon piece (0.7 mm thick) surface, thickness is 200nm,
Two, carbon injects: utilize ion implantation mode that carbon is injected into the nickel film.Ion implantation energy is 600eV, measures to be 5x10
15Cm
-2,
Three, high temperature is scalded fire in order to remove hairs: will inject sample behind the carbon and put into High Temperature Furnaces Heating Apparatus and take off fire, taking off fiery temperature is 1000
oC, taking off the fire time is 15 minutes, vacuum tightness 10
-5Pa.And after taking off fire, reduce to room temperature.So far, the nickel film surface can grow one deck graphene film,
Four, nickel thin film corrosive: have the substrate of graphene film to put into ferric chloride Solution on the surface and corrode, strength of solution is 0.5 mol, and etching time is 24 hours.So far, the nickel film can be corroded fully, and graphene film then can swim in solution surface,
Five, graphene film shifts: with the surface 300nm SiO is arranged
2The silicon substrate of film migrates out the graphene film that swims in solution surface, promptly obtains large-scale graphene film.
Omit detected result.
Claims (2)
1. one kind prepares the method for two-dimensional nano material Graphene on a large scale, it is characterized in that the mode of utilizing the carbon high speed ion to inject provides carbon source to prepare Graphene on a large scale; Concrete steps are as follows:
One, nickel film preparation: adopt sputtering method or pulsed laser deposition method to prepare the nickel film, film thickness between 100-300nm,
Two, carbon injects: the method for utilizing high speed ion to inject, carbon is injected into the surface of nickel film, and ion implantation dosage (Dose) scope is 5x10
15-5x10
16Cm
-2, energy is: 500-1000eV,
Three, high temperature is scalded fire in order to remove hairs: in temperature is to scald fire in order to remove hairs under 600-1000 degree centigrade, and scalding the fire time in order to remove hairs is 15 minutes-60 minutes, and vacuum condition is 10
-5Pa to 1Pa,
Four, nickel thin film corrosive: utilize strength of solution at the iron(ic) chloride of 0.25-1 mol or iron nitrate solution corrosion nickel film, make graphene film swim in solution surface, etching time is at 3-24 hour,
Five, graphene film shifts: utilize any substrate, the graphene film that swims in solution surface is migrated out, promptly obtain large-scale graphene film; So large-scale graphene film just completes, and big I reaches several centimetres.
2. according to the described preparation of claim 1 method of two-dimensional nano material Graphene on a large scale, it is characterized in that described nickel film can be copper or other transiting metal film.
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| CN102655080A (en) * | 2012-05-16 | 2012-09-05 | 西安电子科技大学 | Method for preparing grapheme nanobelt by injecting Si to SiC based on Cu membrane annealing |
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| CN102674332A (en) * | 2012-05-23 | 2012-09-19 | 西安电子科技大学 | Method for preparing structured graphene by reaction of SiC and Cl2 based on Cu film annealing |
| CN102683183A (en) * | 2012-05-16 | 2012-09-19 | 西安电子科技大学 | Preparation method of graphene nanobelt injecting Si to SiC based on Ni film annealing |
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Application publication date: 20110713 |