CN102786049A - System and method for preparing graphene by means of SiC thermal cracking - Google Patents
System and method for preparing graphene by means of SiC thermal cracking Download PDFInfo
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Abstract
The invention relates to a system and a method for preparing graphene by means of SiC thermal cracking. The system comprises a gas-refining quartz tube serving as a vacuum cavity, an SiC substrate, an induction heating graphite boat and a carbon felt heat preservation layer, wherein the SiC substrate is arranged in the middle of the vacuum cavity and in a graphite boat sample groove. The graphite boat is arranged in the middle of the carbon felt heat preservation layer. The carbon felt heat preservation layer is closely attached to the wall of the vacuum cavity to form a hollow structure. One end of the vacuum cavity is provided with a vacuum cavity door used for opening and closing the vacuum cavity. A vacuumizing gas circuit formed by sequentially connecting a baffle valve, a molecular pump and a mechanical pump is arranged below the vacuum cavity door and used for vacuumizing the vacuum cavity according to needs. The other end of the vacuum cavity is provided with an infrared detection window made of glass permeable by infrared rays. The system and the method for preparing graphene by means of SiC thermal cracking have the advantages that high-quality graphene can be prepared at the high barometric-pressure state (0.1-1 barometric pressure).
Description
Technical field
The present invention relates to the technology of preparing of Graphene.
Background technology
Graphene is made up of the two-dimentional novel material of hexagonal structure carbon atom; After An Deliehaimu of University of Manchester in 2004 and Constantine Nuo Woxiaoluofu find; Cause whole world sensation, therefore An Deliehaimu and Constantine Nuo Woxiaoluofu have also obtained Nobel Prize in physics in 2010.Graphene has electronic mobility the highest in the present all material and maximum loaded current density, also has the bipolarity field-effect simultaneously, can realize the continuous modulation from the N type from the P type.Therefore all has good military and civilian prospect aspect millimeter wave, the Terahertz device.In numerous graphene preparation methods such as mechanically peel method, chemical Vapor deposition process, chemical method and SiC pyrolysis method; Because have epitaxy, lattice defect is few, area is big, quality is high; With existing planar S i process compatible; Numerous advantages such as preparation and good process repeatability that can realize the wafer scale fet array make the SiC pyrolysis method show one's talent at microelectronic, but the equipment that is used for the SiC pyrolysis method of the prior art is all immature.
At present, domestic some research institution adopts the SiC thermo-cracking system of molecular beam epitaxy system (MBE) instead of dedicated to carry out the research of epitaxial graphite alkene.Some shortcomings below it exists: 1. owing to the natural characteristics of MBE system, must remain on the environment work down of ultrahigh vacuum(HHV), can't be at growing epitaxial Graphene under the argon shield, the epitaxial graphite alkene quality that therefore grows is unsatisfactory.2.SiC substrate need carry out etching processing with hydrogen before thermo-cracking, remove the left cut of its surface finish, makes it show out step-like atomic-level flatness surface, for the growth of epitaxial graphite alkene provides surface of good.Yet the MBE system can't realize the etching and the growth of original position.The SiC surface is polluted easily in the process of ex situ growth, thereby has influence on the growth quality of Graphene
Summary of the invention
The objective of the invention is deficiency, proposed system and method thereof that the SiC pyrolysis method prepares Graphene for existing Graphene technology of preparing.
One of technical scheme of the present invention: the SiC pyrolysis method prepares the system of Graphene; Comprise a gas refining silica tube as vacuum cavity; Be positioned at .SiC substrate, induction heating graphite boat and the carbon felt thermal insulation layer in vacuum cavity mid-way; Said SiC substrate is positioned at the graphite boat sample cell, and said graphite boat is positioned at carbon felt thermal insulation layer middle part, and said carbon felt thermal insulation layer is close to the tube wall of vacuum cavity and is formed hollow structure;
One end of said vacuum cavity has the vacuum chamber door in order to the opening and closing vacuum cavity, and what below said vacuum chamber door, be connected with flapper valve, molecular pump and mechanical pump composition in turn vacuumizes gas circuit in order to as required vacuum cavity is carried out vacuum pumping; The other end of vacuum cavity has the infrared acquisition window of the outer glass material of red line;
Said load coil is placed in the pairing vacuum cavity tube wall of carbon felt thermal insulation layer and does not contact with the vacuum cavity tube wall outward; Said load coil is connected to form automatic heating feedback circuit with medium frequency induction heater, PID thermostat, infrared temperature measurement device and infrared temperature probe successively, said infrared temperature probe through infrared acquisition window detection sensor heating graphite boat temperature and through infrared temperature measurement device with signal feedback behind the PID temperature controller control medium frequency induction heater and load coil with the control of realization to Heating temperature;
The hydrogen branch road that said sources of hydrogen, hydrogen needle-valve and mass flowmeter are composed in series; The argon gas branch road that said argon gas source, argon gas needle-valve and mass flowmeter are composed in series, said hydrogen branch road and argon gas branch road be the end UNICOM through mass flowmeter and vacuum cavity all; Be linked with the exhaust branch road is made up of by-pass damper valve and the series connection of pumps of bypass machinery in order to the intravital air pressure of control vacuum chamber at the other end of vacuum cavity, the while can also the intravital residual gas of discharge side.
Two of technical scheme of the present invention: the SiC pyrolysis method prepares the method for Graphene, it is characterized in that, comprises the steps:
Step 2. is closed the vacuum chamber door, opens bypass mechanical pump and by-pass damper valve, treats to close the by-pass damper valve after vacuum tightness is lower than 10Pa, opens mechanical pump, flapper valve, molecular pump successively and treats that vacuum tightness is higher than 1 * 10
-5Pa;
Step 4. is closed flapper valve, molecular pump and mechanical pump successively; Open sources of hydrogen, hydrogen needle-valve and by-pass damper valve successively, in vacuum cavity, feed the hydrogen of 500sccm flow and make the intravital pressure of vacuum chamber remain on 0.7 ~ 0.9 normal atmosphere through by-pass damper valve regulation pumping speed;
Step 5. graphite boat temperature under the control of the PID of pre-set program thermostat continues to rise to 1550 ℃ and be incubated 15 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; Insulation naturally cools to room temperature after finishing under hydrogen shield, accomplish the etching of SiC substrate this moment.
Step 6. is closed hydrogen needle-valve and sources of hydrogen, regulates the by-pass damper valve to maximum, treats to close the by-pass damper valve after the intravital vacuum tightness of vacuum chamber is lower than 10Pa, and order is opened mechanical pump, flapper valve and molecular pump and treated that vacuum tightness is higher than 1 * 10
-5Behind the Pa, repeat the 3rd step and discharge the intravital residual gas of vacuum chamber to get rid of;
Step 8. graphite boat temperature under the control of the PID of pre-set program thermostat continues to rise to 1600 ℃ and be incubated 20 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; After insulation finished, the SiC substrate naturally cooled to room temperature under argon shield, accomplished the thermo-cracking growth of epitaxial graphite alkene on the SiC substrate this moment.
The invention has the beneficial effects as follows: adopt system and method for the present invention, can under higher atmospheric pressure state, (0.1～1 normal atmosphere) prepare high-quality Graphene.
Description of drawings
Fig. 1 is a system schematic of the present invention.
Description of reference numerals: gas refining silica tube (vacuum cavity) 1, vacuum chamber door 2, flapper valve 3, molecular pump 4, mechanical pump 5, by-pass damper valve 6, bypass mechanical pump 7, infrared acquisition window 8, SiC substrate 9, induction heating graphite boat 10, carbon felt thermal insulation layer 11, load coil 12, medium frequency induction heater 13, PID thermostat 14, infrared temperature measurement device 15, infrared temperature probe 16, mass flowmeter 17, hydrogen needle-valve 18, argon gas needle-valve 19, argon gas source 20, sources of hydrogen 21.
Embodiment
Below in conjunction with accompanying drawing 1 and specific embodiment specific embodiments of the present invention is done further explanation.
The SiC pyrolysis method prepares the system of Graphene; Comprise a gas refining silica tube 1 as vacuum cavity; Be positioned at .SiC substrate 9, induction heating graphite boat 10 and the carbon felt thermal insulation layer 11 in vacuum cavity mid-way; Said SiC substrate 9 is positioned at graphite boat 10 sample cells, and said graphite boat is positioned at carbon felt thermal insulation layer 11 middle parts, and said carbon felt thermal insulation layer 11 is close to the tube wall of vacuum cavity and is formed hollow structure;
One end of said vacuum cavity has vacuum chamber door 2 in order to the opening and closing vacuum cavity, and what below said vacuum chamber door 2, be connected with flapper valve 3, molecular pump 4 and mechanical pump 5 compositions in turn vacuumizes gas circuit in order to as required vacuum cavity is carried out vacuum pumping; The other end of vacuum cavity has the infrared acquisition window 8 of the outer glass material of red line;
Said load coil 12 is placed in carbon felt thermal insulation layer 11 pairing vacuum cavity tube walls and does not contact with the vacuum cavity tube wall outward; Said load coil 12 is connected to form automatic heating feedback circuit with medium frequency induction heater 13, PID thermostat 14, infrared temperature measurement device 15 and infrared temperature probe 16 successively, and said infrared temperature probe 16 heats graphite boat 10 temperature through infrared acquisition window 8 detection sensors and also through infrared temperature measurement device 15 signal feedback controlled medium frequency induction heaters 13 and load coil 12 to realize the control to Heating temperature to PID temperature controller 14 backs;
The hydrogen branch road that said sources of hydrogen 21, hydrogen needle-valve 18 and mass flowmeter 17 are composed in series; The argon gas branch road that said argon gas source 20, argon gas needle-valve 19 and mass flowmeter 17 are composed in series, said hydrogen branch road and argon gas branch road are all through the end UNICOM of mass flowmeter 17 with vacuum cavity; Be linked with the exhaust branch road that is composed in series by by-pass damper valve 6 and bypass mechanical pump 7 at the other end of vacuum cavity in order to the intravital air pressure of control vacuum chamber, simultaneously can also the intravital residual gas of discharge side.
Above-mentioned hydrogen branch road and argon gas branch road can shared mass flowmeters 17, also can adopt a mass flowmeter 17 separately respectively.
With regard to principle of design; The system of present embodiment comprises three parts: the ultrahigh vacuum cavity body portion of mainly being made up of vacuum cavity; Frequency Induction Heating and the temperature control part mainly formed by automatic heating feedback circuit, main by vacuumizing the gas transport part that gas circuit, exhaust branch road, hydrogen branch road and argon gas branch road are formed.Described ultrahigh vacuum cavity body portion can also be operated under the higher temperature 1000 ℃ when guaranteeing ultrahigh vacuum(HHV).Under the molecular pump and mechanical pump tandem working state of gas transport part, link to each other with cavity through flapper valve, the bypass mechanical pump links to each other with cavity through the by-pass damper valve.Said Frequency Induction Heating and temperature control part, inductive heating element adopts the column graphite boat of graphite material, and load coil is placed in the vacuum cavity outside in the form of a ring, and is not in contact with it.The SiC substrate places in the inner sample cell of graphite boat; The column graphite boat is nested in the open column shape carbon felt and places the interior middle part of silica tube and be positioned at the load coil mid-way; Open column shape carbon felt has guaranteed that also the working temperature of outer quartz pipe is no more than 1000 ℃ when having guaranteed inboard graphite boat comparatively high temps.Load coil is connected with medium frequency induction heater and controlled by the PID temperature controller.Infrared temperature probe through passing through the outer glass material of red line infrared acquisition window detection sensor heating graphite boat temperature and with signal feedback in the PID temperature controller to realize temperature controlling.Said gas transport partly be connected on the mass flowmeter through hydrogen needle-valve, argon gas needle-valve respectively for sources of hydrogen and argon gas source and with vacuum cavity UNICOM.Native system can be operated in 0.1～1 normal atmosphere under the higher atmospheric pressure state, can be operated in again ultra-high vacuum environment (<1 * 10
-5Pa) and higher temperature (800 ~ 1700 ℃).
Adopt said system, corresponding proposition a kind of SiC pyrolysis method prepare the method for Graphene, it is characterized in that, comprise the steps:
Step 2. is closed vacuum chamber door 2, opens bypass mechanical pump 7 and by-pass damper valve 6, treats to close by-pass damper valve 6 after vacuum tightness is lower than 10Pa, opens mechanical pump 5, flapper valve 3, molecular pump 4 successively and treats that vacuum tightness is higher than 1 * 10
-5Pa.
Step 4. is closed flapper valve 3, molecular pump 4 and mechanical pump 5 successively; Open sources of hydrogen 21, hydrogen needle-valve 18 and by-pass damper valve 6 successively, in vacuum cavity, feed the hydrogen of 500sccm flow and make the intravital pressure of vacuum chamber remain on 0.7 ~ 0.9 normal atmosphere through by-pass damper valve 6 adjusting pumping speed.
Step 5. graphite boat 10 temperature under the control of the PID of pre-set program thermostat 14 continue to rise to 1550 ℃ and be incubated 15 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; Insulation naturally cools to room temperature after finishing under hydrogen shield, accomplish the etching of SiC substrate this moment.
Step 6. is closed hydrogen needle-valve 18 and sources of hydrogen 21, regulates by-pass damper valve 6 to maximum, treats to close by-pass damper valve 6 after the intravital vacuum tightness of vacuum chamber is lower than 10Pa, and order is opened mechanical pump 5, flapper valve 3 and molecular pump 4 and treated that vacuum tightness is higher than 1 * 10
-5Behind the Pa, repeat the 3rd step and discharge the intravital residual gas of vacuum chamber to get rid of.
Step 8. graphite boat 10 temperature under the control of the PID of pre-set program thermostat 14 continue to rise to 1600 ℃ and be incubated 20 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; After insulation finished, SiC substrate 9 naturally cooled to room temperature under argon shield, accomplished the thermo-cracking growth of epitaxial graphite alkene on the SiC substrate this moment.
Detect through AFM AFM; The SiC and the epitaxial graphite alkene of being grown that prepare the system and method institute etching of Graphene through above-mentioned SiC pyrolysis method all have good step appearance; Its rootmean-square surfaceness RMS is respectively 0.491nm and 0.410nm, reaches atomic roughness.Through x-ray photoelectron power spectrum XPS detect raising gradually growth temperature under, the number of plies of Graphene also thickens thereupon, the concrete number of plies is 1550 ℃: 1.23 layers, 1580 ℃: 1.55 layers, 1610 ℃: 2.84 layers: 1650 ℃: 4.1 layers.
Those of ordinary skill in the art is to be appreciated that; Above-mentioned each parts such as flapper valve, molecular pump, mechanical pump, PID thermostat and infrared temperature measurement device etc. all can adopt existing ripe element; Therefore do not do detailed description to forming each parts of system that the SiC pyrolysis method prepares Graphene; This does not influence enforcement of the present invention, and the innovative point of native system is the combination utilization to above-mentioned parts.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (2)
1.SiC pyrolysis method prepares the system of Graphene; Comprise a gas refining silica tube as vacuum cavity; Be positioned at SiC substrate, induction heating graphite boat and the carbon felt thermal insulation layer in vacuum cavity mid-way; Said SiC substrate is positioned at the graphite boat sample cell, and said graphite boat is positioned at carbon felt thermal insulation layer middle part, and said carbon felt thermal insulation layer is close to the tube wall of vacuum cavity and is formed hollow structure;
One end of said vacuum cavity has the vacuum chamber door in order to the opening and closing vacuum cavity, and what below said vacuum chamber door, be connected with flapper valve, molecular pump and mechanical pump composition in turn vacuumizes gas circuit in order to as required vacuum cavity is carried out vacuum pumping; The other end of vacuum cavity has the infrared acquisition window of the outer glass material of red line;
Said load coil is placed in the pairing vacuum cavity tube wall of carbon felt thermal insulation layer and does not contact with the vacuum cavity tube wall outward; Said load coil is connected to form automatic heating feedback circuit with medium frequency induction heater, PID thermostat, infrared temperature measurement device and infrared temperature probe successively, said infrared temperature probe through infrared acquisition window detection sensor heating graphite boat temperature and through infrared temperature measurement device with signal feedback behind the PID temperature controller control medium frequency induction heater and load coil with the control of realization to Heating temperature;
The hydrogen branch road that said sources of hydrogen, hydrogen needle-valve and mass flowmeter are composed in series; The argon gas branch road that said argon gas source, argon gas needle-valve and mass flowmeter are composed in series, said hydrogen branch road and argon gas branch road be the end UNICOM through mass flowmeter and vacuum cavity all; Be linked with the exhaust branch road is made up of by-pass damper valve and the series connection of pumps of bypass machinery in order to the intravital air pressure of control vacuum chamber at the other end of vacuum cavity, the while can also the intravital residual gas of discharge side.
2.SiC pyrolysis method prepares the method for Graphene, it is characterized in that, comprises the steps:
Step 1. is positioned over the SiC substrate in the graphite boat sample cell, pushes the gas refining silica tube inside as vacuum cavity from the vacuum chamber door, and places carbon felt thermal insulation layer middle part;
Step 2. is closed the vacuum chamber door, opens bypass mechanical pump and by-pass damper valve, treats to close the by-pass damper valve after vacuum tightness is lower than 10Pa, opens mechanical pump, flapper valve, molecular pump successively and treats that vacuum tightness is higher than 1 * 10
-5Pa;
Step 3. is opened infrared temperature measurement device, PID thermostat and medium frequency induction heater respectively.After making the graphite boat temperature rise to 850 ℃ under the control of the PID of pre-set program thermostat, be incubated 20 minutes to discharge the intravital residual gas of vacuum chamber;
Step 4. is closed flapper valve, molecular pump and mechanical pump successively; Open sources of hydrogen, hydrogen needle-valve and by-pass damper valve successively, in vacuum cavity, feed the hydrogen of 500sccm flow and make the intravital pressure of vacuum chamber remain on 0.7 ~ 0.9 normal atmosphere through by-pass damper valve regulation pumping speed;
Step 5. graphite boat temperature under the control of the PID of pre-set program thermostat continues to rise to 1550 ℃ and be incubated 15 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; Insulation naturally cools to room temperature after finishing under hydrogen shield, accomplish the etching of SiC substrate this moment.
Step 6. is closed hydrogen needle-valve and sources of hydrogen, regulates the by-pass damper valve to maximum, treats to close the by-pass damper valve after the intravital vacuum tightness of vacuum chamber is lower than 10Pa, and order is opened mechanical pump, flapper valve and molecular pump and treated that vacuum tightness is higher than 1 * 10
-5Behind the Pa, repeat the 3rd step and discharge the intravital residual gas of vacuum chamber to get rid of;
Step 7. is closed flapper valve, molecular pump, is reached mechanical pump; Open argon gas source, argon gas needle-valve, reach the by-pass damper valve, in vacuum cavity, feed the argon gas of 100sccm flow and make the intravital pressure of vacuum chamber remain on 0.7 ~ 0.9 normal atmosphere through by-pass damper valve 6 adjusting pumping speed;
Step 8. graphite boat temperature under the control of the PID of pre-set program thermostat continues to rise to 1600 ℃ and be incubated 20 minutes, and whole process vacuum cavity remains on 0.7～0.9 normal atmosphere; After insulation finished, the SiC substrate naturally cooled to room temperature under argon shield, accomplished the thermo-cracking growth of epitaxial graphite alkene on the SiC substrate this moment.
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| CN103130215A (en) * | 2013-03-05 | 2013-06-05 | 电子科技大学 | Silicon surface SiC epitaxial graphene liquid phase fluorine intercalation method |
| CN103641110A (en) * | 2013-12-23 | 2014-03-19 | 福州大学 | Method for preparing graphene by using induction heating |
| CN103864064A (en) * | 2014-03-06 | 2014-06-18 | 新疆大学 | Method for preparing nitrogen-doped graphene |
| CN104695012A (en) * | 2015-03-24 | 2015-06-10 | 山东大学 | Device and method for preparing large-size high-quality graphene single crystal |
| CN104787754A (en) * | 2015-03-19 | 2015-07-22 | 中国科学院物理研究所 | Preparation method of suspended graphene |
| CN105441902A (en) * | 2014-08-12 | 2016-03-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Epitaxial silicon carbide-graphene composite film preparation method |
| CN105717148A (en) * | 2014-12-03 | 2016-06-29 | 天津恒电空间电源有限公司 | Method for measuring layer number of graphene on silicon carbide substrate |
| CN107904659A (en) * | 2017-11-23 | 2018-04-13 | 西北工业大学 | A kind of epitaxial growth equipment of graphene |
| CN109343101A (en) * | 2018-09-11 | 2019-02-15 | 东莞中子科学中心 | Pressure balance control method for white light neutron source charged particle detection spectrometer |
| CN112309810A (en) * | 2019-07-31 | 2021-02-02 | 上海先进半导体制造股份有限公司 | Ion implanter and method and system for monitoring temperature of wafer in real time |
| CN114197039A (en) * | 2021-12-09 | 2022-03-18 | 山东大学 | Method for epitaxially growing uniform graphene more than six inches on 4H-SiC substrate |
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| CN103130215B (en) * | 2013-03-05 | 2014-10-15 | 电子科技大学 | Silicon surface SiC epitaxial graphene liquid phase fluorine intercalation method |
| CN103130215A (en) * | 2013-03-05 | 2013-06-05 | 电子科技大学 | Silicon surface SiC epitaxial graphene liquid phase fluorine intercalation method |
| CN103641110A (en) * | 2013-12-23 | 2014-03-19 | 福州大学 | Method for preparing graphene by using induction heating |
| CN103641110B (en) * | 2013-12-23 | 2016-06-01 | 福州大学 | A kind of method utilizing induction heating to prepare Graphene |
| CN103864064A (en) * | 2014-03-06 | 2014-06-18 | 新疆大学 | Method for preparing nitrogen-doped graphene |
| CN105441902B (en) * | 2014-08-12 | 2018-03-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of preparation method of epitaxial silicon carbide graphene composite film |
| CN105441902A (en) * | 2014-08-12 | 2016-03-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Epitaxial silicon carbide-graphene composite film preparation method |
| CN105717148A (en) * | 2014-12-03 | 2016-06-29 | 天津恒电空间电源有限公司 | Method for measuring layer number of graphene on silicon carbide substrate |
| CN104787754A (en) * | 2015-03-19 | 2015-07-22 | 中国科学院物理研究所 | Preparation method of suspended graphene |
| CN104695012A (en) * | 2015-03-24 | 2015-06-10 | 山东大学 | Device and method for preparing large-size high-quality graphene single crystal |
| CN104695012B (en) * | 2015-03-24 | 2017-03-22 | 山东大学 | Device and method for preparing large-size high-quality graphene single crystal |
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| CN109343101A (en) * | 2018-09-11 | 2019-02-15 | 东莞中子科学中心 | Pressure balance control method for white light neutron source charged particle detection spectrometer |
| CN109343101B (en) * | 2018-09-11 | 2023-03-14 | 东莞中子科学中心 | Differential pressure balance control method for white light neutron source charged particle detection spectrometer |
| CN112309810A (en) * | 2019-07-31 | 2021-02-02 | 上海先进半导体制造股份有限公司 | Ion implanter and method and system for monitoring temperature of wafer in real time |
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