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• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/15—Nano-sized carbon materials
  • C01B32/182—Graphene
  • C01B32/184—Preparation
  • C01B32/186—Preparation by chemical vapour deposition [CVD]
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
  • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
  • C23C16/463—Cooling of the substrate
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y40/00—Manufacture or treatment of nanostructures
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  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/02—Pretreatment of the material to be coated
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
  • C23C16/26—Deposition of carbon only
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
  • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
  • C23C16/54—Apparatus specially adapted for continuous coating
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
  • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
  • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
  • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
  • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation

Definitions

• the present invention relates to the production of graphene on copper at atmospheric pressure with modified chemical vapor deposition (AP-CVD). More specifically, a method and system for producing graphene on a copper substrate by modified chemical vapor deposition (AP-CVD).
• AP-CVD modified chemical vapor deposition
• Patent application US2013217222 dated 22.08.2013 entitled “Large-scale graphene sheet: articles, compositions, methods and devices incorporating them", by Johnson et al., Describes methods for large-scale cultivation of uniform graphene layers on flattened substrates using chemical vapor deposition (CVD) at atmospheric pressure (AP); Graphene is produced according to these methods, it can have a single layer content less than or equal to 95%.
• Field effect transistors manufactured by the process of the invention have hole mobilities at room temperature that are a factor of 2 to 5 larger than the media for samples grown on commercially available copper foil substrates.
• Patent application WO2014174133 dated 30.10.2014 entitled “Method for the controlled production of graphene under a very low environment pressure and device for obtaining it ", by Bertrán Serra Enric and others, describes a method and a device for preparing a graphene structure of 1-5 layers, the control of the number of layers, by means of a chemical vapor deposition method (CVD) on a pre-determined substrate, at a vacuum pressure of 10 "4 - 10 " 5 Pa, the temperature being between 500 -1050 ° C, based on the use of a carbon precursor gas with a synchronized sequence of pulses
• Each pulse has a specific escape time for the precursor gas, as a result of pumping, the pressure pulse consisting of an increase in instantaneous pressure as a result of the instantaneous opening of a valve, followed by a decrease in the exponential pressure, the number of pulses depending on the number of layers, and the time between pulses according to the specific escape time of the carbon precursor gas.
• Patent application WO2012031238, dated 08.03.2012 entitled “Uniform multilayers of graphene by chemical vapor deposition", by Zhoug Zhaohui et al., Describes a uniform multilayer graphene production method by Deposition Steam Chemistry (CVD).
• the method is limited in size only by the size of the CVD reaction chamber and is scalable to produce multilayer graphene films on a wafer scale that have the same number of graphene layers throughout substantially the entire film.
• Uniform bilayer graphene can be produced using a method that does not require mounting single-layer graphene produced independently.
• the method includes a CVD process, in which a reaction gas is flowed in the chamber at a relatively low pressure compared to conventional processes and the temperature in the reaction chamber decreased relatively slowly compared to the conventional processes
• a first objective of the invention is a method for producing graphene on a copper substrate by modified chemical vapor deposition (AP-CVD), comprising:
• an open chamber which is constituted by a cylindrical glass chamber, where its axial axis is oriented vertically, where the cylindrical glass chamber is fully open on its lower face;
• Electromagnetic induction is 1000 ° C; and the two circular copper sheets, arranged inside the cylindrical glass chamber, are 30 mm in diameter and 0.1 mm thick with a purity of 99.8%; They are also located in separate parallel forms and supported by three ceramic pillars 3.5 mm in diameter and 30 mm long, which are also subject to a base of the same material.
• the electromagnetic induction heater consisting of a coil, preferably 2.5 ⁇ - ⁇ , which is wound externally to the cylindrical glass chamber, where the coil is fed by an alternating current generated by a frequency oscillator, preferably at 250 KHz; Prior to the introduction of the two copper sheets to the glass cylindrical chamber, they are treated with acetic acid for 2 minutes and rinsed with ethanol. In addition, the copper sheets are kept under Methane and Argon flows of 1.0 L / min and 0.1 L / min, respectively, for 2 minutes, and with the same flows of Methane and Argon are cooled, with a reduction Cooling is from 1000 ° C to 600 ° C in about 5 seconds. The default time to heat to around 1000 ° C, through the electromagnetic induction heater is 15 minutes.
• the material of the glass cylindrical chamber is preferably Pyrex, 40 mm in diameter and 110 mm long.
• a second objective of the invention is a system for producing graphene on a copper substrate by modified chemical vapor deposition (AP-CVD), which comprises two copper sheets arranged in parallel and separated with a ceramic material; said two copper sheets are incorporated into an open chamber, which is constituted by a cylindrical glass chamber, where its axial axis is oriented vertically, where the cylindrical glass chamber is fully open in its lower face; an electromagnetic induction heater at a predetermined temperature, to heat the two copper sheets and for a predetermined time; a supply of a mixture of methane and argon flow rates on the upper face of said cylindrical glass chamber; and a radiation pyrometer to continuously monitor the temperature of the two copper sheets through a window of Quartz arranged on the upper face of the cylindrical glass chamber.
• AP-CVD modified chemical vapor deposition
• Figure 1 describes a scheme of the system of the present invention.
• Figure 2 describes an arrangement of the copper sheets of the graphene synthesis of the present invention; with the Raman 532 nm spectra obtained directly on the inner and outer faces of the copper sheets of the synthesis of the present invention.
• Figure 3 describes the Raman 514 nm spectrum of graphene grown on one of the inner copper sheets.
• Figure 4 describes micrographs of graphene transferred to silicon oxide, where regions of mono and bilayers of graphene are observed according to Raman 532 nm spectra.
• Figure 5 describes Raman spectra with wavelength 647 nm of graphene grown on one of the copper sheets, internal face and transferred on a Si0 2 / Si substrate.
• Figure 6 describes the 488 nm Raman spectrum of graphene on one of the inner copper plates.
• Figure 7 describes the Raman 514 nm spectrum of graphene grown on one of the copper sheets, internal face and transferred to Si0 2 / Si at ten different points of the radial direction substrate.
• Figure 8 shows the variation of the exposure time of the sheets as a function of 2D / G and abbreviated average height width FWHM (Full Width at Half Maximum).
• Figure 9 shows the temperature variation of the as a function of 2D / G FWHM.
• Figure 10 shows the variation of the separation distance of the sheets in the synthesis, as a function of 2D / G, D / G and in the insert the curve "b" as a function of the FWHM.
• the synthesis of graphene is carried out in a single step, in an open chamber without the addition of gaseous hydrogen using only argon and methane, in addition, at the end of the synthesis the system quickly reaches the conditions for A new graphene growth process.
• the present invention produces graphene by means of a novel configuration of the substrate which is constituted by two copper sheets (40) arranged in parallel and separated with ceramic material (30) which are heated via electromagnetic induction (20) to a 1000 ° C temperature.
• the space formed between plates or interfacial zone retains the species of decomposition, hydrogen and intermediate species which inhibit the action of residual oxygen and reduce the native oxide of the surface of Cu in that area, in addition, these species favor the adsorption of the carbon achieving the growth of graphene on the inner faces of the sheets.
• the system for producing graphene (100) in AP-CVD in open chamber shown in Figure 1, consists of a cylindrical glass chamber (10), preferably Pyrex with 40 mm diameter and 110 mm long, where its axial axis is It is oriented vertically, the cylindrical glass chamber (10) is fully open on its lower face (15) and on its upper face (18) a mixture of Methane and Argon is supplied.
• a cylindrical glass chamber (10) preferably Pyrex with 40 mm diameter and 110 mm long, where its axial axis is It is oriented vertically, the cylindrical glass chamber (10) is fully open on its lower face (15) and on its upper face (18) a mixture of Methane and Argon is supplied.
• the two copper sheets (40) are heated via electromagnetic induction through an electromagnetic induction heater (20) consisting of a coil, preferably 2.5 ⁇ - ⁇ that is wound externally to the cylindrical chamber of glass (10), where the coil of the electromagnetic induction heater (20) is powered by an alternating current generated by a frequency oscillator (not shown), preferably equal to 250 KHz. This frequency is chosen due to the high electrical conductivity of the circular copper sheets (40).
• an electromagnetic induction heater (20) consisting of a coil, preferably 2.5 ⁇ - ⁇ that is wound externally to the cylindrical chamber of glass (10), where the coil of the electromagnetic induction heater (20) is powered by an alternating current generated by a frequency oscillator (not shown), preferably equal to 250 KHz. This frequency is chosen due to the high electrical conductivity of the circular copper sheets (40).
• the temperature of the two copper sheets (40) is continuously monitored by a radiation pyrometer (50) through a quartz window (60) arranged on the upper face (18) of the glass cylindrical chamber ( 10), thus it is possible to control the temperature through the supply of the electromagnetic induction heater (20).
• the copper sheets (40) Prior to the introduction of the two copper sheets (40) into the cylindrical glass chamber (10), these are treated with acetic acid for 2 minutes and rinsed with ethanol, thus in the cylindrical glass chamber (10) , the copper sheets (40) are kept under argon and methane flow rates of 1.0 L / min and 0.1 L / min, respectively, for 2 minutes, then they are heated to about 1000 ° C through the Electromagnetic induction heater (20) for 15 minutes, at the end of this stage, it is left cool with the same argon and methane flow rates, to room temperature achieving a cooling of 1000 ° C to 600 ° C for about 5 seconds.
• Raman spectroscopy is a powerful non-destructive technique widely used for the identification and characterization of graphene and carbon-based materials.
• the features that stand out in the Raman spectrum of graphene are the band D-1350 cm-1, D * -1622 cm-1, G ⁇ 1580 cm-1 and 2D-2700 cm-1.
• the G band is related to the stretching movement of the sp2 links, the D and D * bands are associated with induced defect, and finally the 2D band that is an over tone of the D band, which is useful for specifying the number of graphene layers.
• the ratio between D / G intensities is widely used to characterize graphene defects.
• the ratio of 2D / G intensities is a measure of the number of graphene layers. For mono graphene layer the ratio is greater than 2.
• Graphene obtained through the present invention is identified and characterized with Raman spectrometer at wavelengths of 514, 532 and 647 nm.
• FIG. 4 A micrograph of the graphene surface transferred to a substrate of SI0 2 / Si is shown in Figure 4, with regions of monolayer and bilayer of graphene being observed according to their Raman spectra in the insert.
• Figure 6 shows the typical Raman spectrum of graphene, obtained directly on one of the copper sheets in the inter-facial zone with Raman spectrometer of 514 nm.
• Figure 7 shows the photograph of some of the sheets exposed to the synthesis on their inner face, which is then transferred to the grown graphene, to a substrate of SI0 2 / Si, from which the Raman spectra were obtained in ten places different in radial direction.
• Figure 8 shows the variation of the exposure time of the sheets as a function of 2D / G and FWHM where the synthesis parameters are: separation distance between sheets of 1 mm, temperature of 970 ° C and flow rates of 1 and 0.1 L / min of argon and methane respectively.
• the 532nm Raman spectra are directly obtained in one of the copper sheets of copper inner copper face in nine different places, obtaining their respective 2D / G, D / G and FWHM ratios that are finally averaged, observing an optimal synthesis time around 15 min.
• Figure 9 shows the temperature variation of the functions as a function of 2D / G and FWHM, where the synthesis parameters are: exposure time 10 min, separation distance between sheets of 1 mm and flow rates of 1 and 0.1 L / min of argon and methane respectively.
• Raman spectra of 532 nm are directly obtained in one of the inner face copper sheets in nine different locations, obtaining their respective 2D / G, D / G and medium height width (FWHM) ratios, which are finally averaged. Observing an optimum temperature of the synthesis around 970 ° C.
• Figure 10 in curves "a” shows the variation of the distance in the separation of the sheets in the synthesis, as a function of 2D / G, D / G and in the curve insert "b" figure 10 as a function of FWHM where the synthesis exposure times are 10 min, synthesis temperature of 970 ° C and flow rates of 1 and 0.1 L / min of argon and methane respectively.
• the Raman spectra of 532 nm are directly obtained in one of the inner face copper sheets in nine different places, obtaining their respective 2D / G, D / G and FWHM ratios that are finally averaged, observing an optimal separation distance around 1 mm

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