CN103373721A - Method for treating graphene on inert base - Google Patents
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- CN103373721A CN103373721A CN2012101074751A CN201210107475A CN103373721A CN 103373721 A CN103373721 A CN 103373721A CN 2012101074751 A CN2012101074751 A CN 2012101074751A CN 201210107475 A CN201210107475 A CN 201210107475A CN 103373721 A CN103373721 A CN 103373721A
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Abstract
The invention discloses a method for treating graphene on an inert base. The method only comprises a step of immersing graphene in an aqueous solution with a hydrogen ion concentration of 8-10 mol/L and a Mn2O7 concentration of 0.016-0.4wt%; therefore, the method is simple and low in consumption; since graphene with different electrical properties can be obtained through adjusting the immersing time, the method is controllable; and the method needs mild reaction conditions and can be performed at room temperature without stirring, thereby implementing the treatment of graphene on an inert base. The method disclosed by the invention can be widely applied to industrial production.
Description
Technical field
The present invention relates to a kind of method of processing Graphene, be specifically related to a kind of method of processing Graphene in the inertia substrate.
Background technology
Since be found in 2004 can stable existence since, Graphene becomes the focus of scientific circles and industry member because of its perfect crystalline structure and unique physicochemical property such as mechanics, optics, electricity and calorifics.Graphene is the carbonaceous material by the bi-dimensional cellular shape crystalline structure of the tightly packed one-tenth of monolayer carbon atom, is the thinnest known a kind of material.It has higher carrier mobility, can reach 2 * 10
5Cm
2v
-1s
-1, its value is about 100 times of the traditional silicon material, and at room temperature has micron-sized mean free path, therefore has potentiality and replaces the core material that silicon becomes semiconductor element of future generation.
Yet in the situation of intrinsic state, Graphene is zero gap semiconductor, and can't regulate concentration, type and the flow direction of its current carrier.But for the microelectronics industry of reality, the motion of electric current has important practical significance in the induced material, such as the application of the wire in the circuit and quantum device application etc.Therefore, electrical properties how effectively to control Graphene makes it to be applicable to different types of device application, is determining that this novel material is in the development prospect of semicon industry.The electrical properties of Graphene generally comprises the specific targets such as specific conductivity, doping level and energy gap.
At present, scientists mainly reaches the purpose that changes its electrical properties by the mode of the intrinsic Graphene being modified processing.Type by treatment process mainly can be divided into following two large classes:
Physical regulating: namely utilize the physics means, do not destroying Graphene intrinsic sp
2In the situation of carbon structure, its electronic structure is modified.Can be divided into quantum confined effect, electrostatic field regulation and control and stress regulation and control according to mechanism of action difference.But physical method is mainly relied in micro-processing technology, is achieved regulation and control to the Graphene electrical properties by the mode of constructing electron device, and making processes is comparatively complicated, and energy consumption is larger relatively, is unsuitable for the application of industry member and popularizes.
Chemical doping: namely utilize chemical process, utilize foreign atom to replace the originally carbon atom on lattice, or produce new chemical functional group with carbon atom generation chemical reaction, and then affect the sp of carbon atom
2Hybridized orbital changes its electronic structure.Chemical doping is because of its foreign atom diversity, and the physico-chemical property of the Graphene derivative of formation becomes the focus of research gradually than horn of plenty.
The method of chemical doping Graphene mainly is divided into following several at present:
Gas phase etching method: mainly be to utilize the gaseous phase free radical with high reaction activity that the Graphene surface is bombarded, or at high temperature allow gas molecule and Graphene react.At present, the method for Graphene by oxygen, hydrogen, ammonia doping there has been widely research.But this method need to be introduced the reaction unit with high vacuum system, and causes easily the structure deteriorate of irrecoverability on the Graphene surface, therefore not too is applicable to actual heavy industrialization processing.
Liquid phase is modified method: mainly be to utilize solution reaction, Graphene and derivative and the interaction of other active substances with having disperseed in solution generate new Graphene derivative.Because the partial reaction condition is comparatively fierce, need in the situation of high temperature or low temperature stirring, carry out, it generally is for the Graphene that has disperseed in organic or inorganic solution and derivative thereof that solution method is mixed.And for the relevant industry of electron device, grow or the Graphene that is deposited in the inertia substrate (such as silicon-dioxide) then is the object of main researchdevelopment.
Therefore, the application in microelectronic industry has important practical significance to this brand-new material to develop the method for Graphene in convenient, the low consumption of a cover, the controlled processing inertia substrate.
Summary of the invention
The objective of the invention is in order to overcome defects of the prior art, the method for Graphene in a kind of new processing inertia substrate is provided.
The present inventor is unexpected under study for action to find that it is 8-10mol/L and Mn that Graphene is immersed in hydrogen ion concentration
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight, need not high temperature or low temperature and stirs the electrical properties that can effectively control Graphene, therefore is applicable to process be positioned at the suprabasil Graphene of inertia.
Therefore, to achieve these goals, the invention provides a kind of method of processing Graphene in the inertia substrate, the method comprises: it is 8-10mol/L and Mn that Graphene is immersed in hydrogen ion concentration
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight.
Preferably, hydrogen ion concentration is 8.7-9.1mol/L, Mn
2O
7Concentration is the 0.04-0.2 % by weight.
Preferably, described hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is that the aqueous solution of 0.016-0.4 % by weight is the H of 45-52 % by weight by concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.05-1.2 % by weight
4The aqueous solution obtains with volume ratio 1: 0.9-1.1 reaction.
Preferably, be 8-10mol/L and Mn Graphene being immersed in hydrogen ion concentration
2O
7Concentration be in the aqueous solution of 0.016-0.4 % by weight before, the method also comprises carries out following processing to Graphene:
(1) on the Graphene surface polymer materials is set, this polymer materials can protect Graphene not oxidized;
The part that (2) will be arranged on the polymer materials on Graphene surface is got rid of, to expose the Graphene of part.
The method of Graphene in the processing inertia provided by the invention substrate, only needing Graphene is immersed in hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight, and method is simple, low consumption; Can immerse the Graphene that the time obtains different electrical properties by adjusting, method is controlled; Reaction conditions is gentle, at room temperature can carry out, and need not to stir, and has realized being positioned at the processing of the suprabasil Graphene of inertia.The inventive method can be widely used in industrial production.
Other features and advantages of the present invention will partly be described in detail in embodiment subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that embodiment described herein only is used for description and interpretation the present invention, is not limited to the present invention.
The invention provides a kind of method of processing Graphene in the inertia substrate, the method comprises: it is 8-10mol/L and Mn that Graphene is immersed in hydrogen ion concentration
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight.
According to the present invention, be 8-10mol/L and Mn although Graphene is immersed in hydrogen ion concentration
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight, can realize purpose of the present invention, i.e. convenient, low consumption, the controlled suprabasil Graphene of processing inertia are to change the electrical properties of Graphene.But it will be understood by those skilled in the art that Mn
2O
7Concentration is higher, and the speed of processing Graphene is faster, and namely the variation of the electrical properties of Graphene is faster, inconvenience is controllably processed, therefore, and for controlled processing Graphene better, namely further improve the controllability of the inventive method, hydrogen ion concentration is preferably 8.7-9.1mol/L, Mn
2O
7Concentration is preferably the 0.04-0.2 % by weight.
Among the present invention, because being positioned at the suprabasil Graphene of inertia is single-layer graphene, namely be that one deck forms the flat film that hexangle type is the honeycomb lattice by carbon atom with the sp2 hybridized orbital, only has a carbon atom thickness, therefore, being difficult to weight or meausurement sign Graphene and hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is the amount ratio of the aqueous solution of 0.016-0.4 % by weight, and hydrogen ion concentration is 8-10mol/L and Mn
2O
7As long as being the consumption of the aqueous solution of 0.016-0.4 % by weight, concentration Graphene can be immersed wherein.
Among the present invention, be 8-10mol/L and Mn for hydrogen ion concentration
2O
7Concentration be the source of the aqueous solution of 0.016-0.4 % by weight without particular requirement, can adopt this area the whole bag of tricks commonly used to obtain, from Mn easy to operate and that obtain
2O
7The aqueous solution considers that to the aspect that Graphene has no adverse effect hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is that the aqueous solution of 0.016-0.4 % by weight preferably is the H of 45-52 % by weight by concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.05-1.2 % by weight
4The aqueous solution obtains with volume ratio 1: 0.9-1.1 reaction; Further preferred is the H of 46-48 % by weight by concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.12-0.48 % by weight
4The aqueous solution obtains with volume ratio 1: 0.96-1.04 reaction, to obtain hydrogen ion and Mn
2O
7Preferred concentration range for, namely obtaining hydrogen ion concentration is 8.7-9.1mol/L and Mn
2O
7Concentration is the aqueous solution of 0.04-0.2 % by weight.
Among the present invention,, at room temperature can carry out without particular requirement for the condition of immersing, so temperature is preferably 10-30 ℃; For immersing the time, the time is too short, and electrical properties changes very little, without too large practical significance, overlong time, electrical properties does not change substantially, and production capacity reduces, therefore, time is preferably 1-3600 second, more preferably 5-1800 second, further is preferably 10-600 second.
In addition, it will be understood by those skilled in the art that in immersing process that the specific conductivity of Graphene reduces gradually, Graphene is the direction doping in hole towards current carrier, immerses certain hour, and the energy gap of Graphene just can be opened, and edge energy just can change.According to the present invention, after Graphene immersed, the electrical properties of Real-Time Monitoring Graphene, with reference to monitoring result, the application needs according to different immerse the different time with Graphene, obtain the Graphene of required electrical properties, namely are controlled described in the present invention.
Among the present invention, the method preferably also comprises: the Graphene after will immersing contacts with deionized water, remains in Mn on the Graphene with flush away
2O
7The aqueous solution.In order not affect the electrical properties of the Graphene after immersing, the resistance value of deionized water is preferably 10-18.2M Ω, more preferably 15-18.2M Ω.Without particular requirement, can adopt this area variety of way commonly used for the mode that contacts with deionized water, the Graphene after for example will immersing is transferred in the deionized water, leaves standstill 3-5min.It will be understood by those skilled in the art that with the Graphene after the washed with de-ionized water for direct application, the Graphene after can will cleaning with nitrogen dries up.
Among the present invention, modifying processing for Graphene being carried out patterning, be applied to the manufacturing of industrialization logical circuit, is 8-10mol/L and Mn Graphene being immersed in hydrogen ion concentration
2O
7Concentration be in the aqueous solution of 0.016-0.4 % by weight before, the method preferably also comprises carries out following processing to Graphene:
(1) on the Graphene surface polymer materials is set, this polymer materials can protect Graphene not oxidized;
The part that (2) will be arranged on the polymer materials on Graphene surface is got rid of, to expose the Graphene of part.
Among the present invention, can be that commonly use in this area various can be protected the not oxidized polymer materials of Graphene for polymer materials, for example be PMMA.For the thickness that polymer materials arranges, as long as can protect Graphene not oxidized, if for example polymer materials is PMMA, the thickness of setting is preferably 100-500nm, more preferably 200-400nm.Without particular requirement, can adopt this area variety of way commonly used, for example spin coating for the mode that arranges.
Among the present invention, a part that is arranged on the polymer materials on Graphene surface is got rid of, to expose the Graphene of part, namely be the polymer materials that is arranged on the Graphene surface to be carried out patterning form window, the place exposes Graphene at window, patterning is generally micron order, can adopt this area various micro-processing methods commonly used, for example electron beam exposure or photoengraving for the mode of patterning; For the window that patterning forms, can form as required the window of various patterns.Behind the formation window Graphene being immersed in hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is to process in the aqueous solution of 0.016-0.4 % by weight, and treatment process does not repeat them here as mentioned before.
Among the present invention, after the Graphene that forms window processed, after the Graphene that is about to form window immerses, preferably also comprise the polymer materials on the Graphene is got rid of.Without particular requirement, can adopt this area variety of way commonly used for the mode that the polymer materials on the Graphene is got rid of, when for example polymer materials is PMMA, can the PMMA on the Graphene be dissolved with acetone, and dry up with nitrogen.
Among the present invention, form the Graphene of window, after processing, namely after immersing, relate to deionized water and contacting, remain in Mn on the Graphene with flush away
2O
7The aqueous solution, also relate to the polymer materials on the Graphene got rid of, for the sequencing of this two step, it should be appreciated by those skilled in the art, the window that forms in order not destroy patterning should be that Graphene contacts with deionized water first, remains in Mn on the Graphene with flush away
2O
7The aqueous solution, and then the polymer materials on the Graphene got rid of.
Among the present invention, without particular requirement, can for this area various inertia substrates commonly used, for example can for silicon-dioxide, silicon nitride or boron nitride, be preferably silicon-dioxide for the inertia substrate.
It will be understood by those skilled in the art that being positioned at the suprabasil Graphene of inertia is single-layer graphene, namely be one deck by carbon atom with sp
2Hybridized orbital forms the flat film that hexangle type is the honeycomb lattice, only has a carbon atom thickness.The inventive method can be processed the powder that obtains after the Graphene pulverizing equally.
More than describe preferred implementation of the present invention in detail; but the present invention is not limited to the detail in the above-mentioned embodiment, in technical conceive scope of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Need to prove in addition, each concrete technical characterictic described in above-mentioned embodiment in reconcilable situation, can make up by any suitable mode, for fear of unnecessary repetition, the present invention is to the no longer separately explanation of various possible array modes.
In addition, also can carry out arbitrary combination between the various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Embodiment
Following embodiment will the present invention is further illustrated, but therefore do not limit the present invention.
In the following embodiments:
The measuring method of specific conductivity: utilize micro-processing technology to construct the graphene field effect transistor of standard, by the fixed gate magnitude of voltage, measure the leakage current value under different drain voltage conditions.The electricity that obtains Graphene under fixed gate voltage by calculating slope that leakage current changes straight line with drain voltage is led.Determined again length and the width of Graphene in the graphene field effect transistor by electron microscope, by Conductivity Calculation formula (specific conductivity=(electricity is led * length)/cross-sectional area, wherein, cross-sectional area=width * carbon atom height) obtain the specific conductivity of Graphene under fixed gate voltage, used gate voltage is the gate voltage at the dirac point place of Graphene in the present embodiment.
The measuring method of energy gap: the measurement by the microcell Raman spectrum can obtain the Raman line of Graphene under the 514nm excitation wavelength, and then (wave number is 1582cm to obtain processing the G peak of rear Graphene
-1) and (wave number is 1350cm at the D peak
-1) raman characteristic peak.Can obtain its peak height ratios (ID/IG) by the peak height that compares D peak and G peak.By the TK relational expression (pass to (ID/IG) and treatment time is tied to form figure: as (ID/IG) when increasing along with the growth in treatment time, the ID/IG=4.4/ characteristic length; As (ID/IG) when reducing along with the growth in treatment time, ID/IG=0.55 * (characteristic length) 2) and quantum confined effect (energy gap ≈ 2/ characteristic length) can extrapolate process after the edge energy of Graphene.
Embodiment 1
Be the H of 47.4 % by weight with concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.237 % by weight
4The aqueous solution is mixed to get Mn with volume ratio at 1: 1
2O
7The aqueous solution, calculate Mn
2O
7Concentration be 0.08325 % by weight, measure Mn
2O
7The aqueous solution in hydrogen ion concentration be 9.1mol/L.Under 20 ℃, the silicon-dioxide substrate that deposits Graphene is immersed in the Mn that obtains
2O
7The aqueous solution in.Respectively when immersing 0s, 10s, 20s, 40s, 90s, 180s, 360s, 600s, with substrate from Mn
2O
7The aqueous solution in take out, be transferred in the deionized water that resistance value is 18.2M Ω, leave standstill 4min, then take out and dry up with nitrogen.Mensuration is immersed specific conductivity and the energy gap of the Graphene behind the different time, the results are shown in Table 1.
Embodiment 2
Be the H of 46.6 % by weight with concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.131 % by weight
4The aqueous solution is mixed to get Mn with volume ratio at 1: 0.96
2O
7The aqueous solution, calculate Mn
2O
7Concentration be 0.045 % by weight, measure Mn
2O
7The hydrogen ion concentration of the aqueous solution be 8.9mol/L.Under 10 ℃, the silicon-dioxide substrate that deposits Graphene is immersed in the Mn that obtains
2O
7The aqueous solution in.Respectively when immersing 0s, 10s, 20s, 40s, 90s, 180s, 360s, 600s, with substrate from Mn
2O
7The aqueous solution in take out, be transferred in the deionized water that resistance value is 15.2M Ω, leave standstill 3min, then take out and dry up with nitrogen.Mensuration is immersed specific conductivity and the energy gap of the Graphene behind the different time, the results are shown in Table 1.
Embodiment 3
Be the H of 48 % by weight with concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.472 % by weight
4The aqueous solution is mixed to get Mn with volume ratio at 1: 1.04
2O
7The aqueous solution, calculate Mn
2O
7Concentration be 0.169 % by weight, measure Mn
2O
7The hydrogen ion concentration of the aqueous solution be 8.7mol/L.Under 30 ℃, the silicon-dioxide substrate that deposits Graphene is immersed in the Mn that obtains
2O
7The aqueous solution in.Respectively when immersing 0s, 10s, 20s, 40s, 90s, 180s, 360s, 600s, with substrate from Mn
2O
7The aqueous solution in take out, be transferred in the deionized water that resistance value is 17M Ω, leave standstill 5min, then take out and dry up with nitrogen.Mensuration is immersed specific conductivity and the energy gap of the Graphene behind the different time, the results are shown in Table 1.
Embodiment 4
Be the H of 51.6 % by weight with concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.95 % by weight
4The aqueous solution is mixed to get Mn with volume ratio at 1: 1.1
2O
7The aqueous solution, calculate Mn
2O
7Concentration be 0.35 % by weight, measure Mn
2O
7The hydrogen ion concentration of the aqueous solution be 9.5mol/L.Under 30 ℃, the silicon-dioxide substrate that deposits Graphene is immersed in the Mn that obtains
2O
7The aqueous solution in.Respectively when immersing 0s, 10s, 20s, 40s, 90s, 180s, 360s, 600s, with substrate from Mn
2O
7The aqueous solution in take out, be transferred in the deionized water that resistance value is 17M Ω, leave standstill 5min, then take out and dry up with nitrogen.Mensuration is immersed specific conductivity and the energy gap of the Graphene behind the different time, the results are shown in Table 1.
Table 1
Annotate: "-" expression Graphene energy gap is not also opened, without edge energy.
As can be seen from Table 1, the inventive method can change the electrical properties of Graphene in the inertia substrate, and can controllably process according to the time of immersing and be positioned at the suprabasil Graphene of inertia.
Embodiment 1-3 and embodiment 4 compared to find out Mn
2O
7Concentration high, the change in electrical properties of Graphene is very fast, inconvenience is controllably processed, namely the method controllability is relatively poor, hydrogen ion concentration is 8.7-9.1mol/L and Mn
2O
7Concentration is that the aqueous solution of 0.04-0.2 % by weight is better to the controllability of Graphene processing.
The method of Graphene in the processing inertia provided by the invention substrate, only needing Graphene is immersed in hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight, and method is simple, low consumption; Can immerse the Graphene that the time obtains different electrical properties by adjusting, method is controlled; Reaction conditions is gentle, at room temperature can carry out, and need not to stir, and has realized being positioned at the processing of the suprabasil Graphene of inertia.The inventive method can be widely used in industrial production.
Claims (10)
1. method of processing Graphene in the inertia substrate, the method comprises: it is 8-10mol/L and Mn that Graphene is immersed in hydrogen ion concentration
2O
7Concentration is in the aqueous solution of 0.016-0.4 % by weight.
2. method according to claim 1, wherein, hydrogen ion concentration is 8.7-9.1mol/L, Mn
2O
7Concentration is the 0.04-0.2 % by weight.
3. method according to claim 1, wherein, described hydrogen ion concentration is 8-10mol/L and Mn
2O
7Concentration is that the aqueous solution of 0.016-0.4 % by weight is the H of 45-52 % by weight by concentration
2SO
4The aqueous solution and concentration are the KMnO of 0.05-1.2 % by weight
4The aqueous solution obtains with volume ratio 1: 0.9-1.1 reaction.
4. method according to claim 1 and 2, wherein, the described condition of immersing comprises: temperature is 10-30 ℃, the time is 1-3600 second.
5. method according to claim 1 and 2, wherein, the method also comprises: the Graphene after will immersing contacts with deionized water, remains in Mn on the Graphene with flush away
2O
7The aqueous solution.
6. method according to claim 5, wherein, the resistance value of described deionized water is 10-18.2M Ω.
7. method according to claim 1 and 2 wherein, is 8-10mol/L and Mn Graphene being immersed in hydrogen ion concentration
2O
7Concentration be in the aqueous solution of 0.016-0.4 % by weight before, the method also comprises carries out following processing to Graphene:
(1) on the Graphene surface polymer materials is set, this polymer materials can protect Graphene not oxidized;
The part that (2) will be arranged on the polymer materials on Graphene surface is got rid of, to expose the Graphene of part.
8. method according to claim 7, wherein, described polymer materials is PMMA, the thickness of setting is 100-500nm.
9. method according to claim 7, wherein, described method also comprises gets rid of the polymer materials on the Graphene after immersing.
10. method according to claim 1 and 2, wherein, described inertia substrate is silicon-dioxide, silicon nitride or boron nitride.
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