CN106145103A - A kind of preparation method of two-dimensional layer hetero-junctions based on Graphene - Google Patents
A kind of preparation method of two-dimensional layer hetero-junctions based on Graphene Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of two-dimensional layer hetero-junctions based on Graphene.This preparation method comprises the steps: 1) it is passed through hydrogen and carbon source gas by being placed with in the reaction chamber of metallic substrates, and heat described reaction chamber and make carbon dissolution in described metallic substrates；2) stop in described reaction chamber, be passed through described carbon source gas, and reacting by heating source makes it grow in described metallic substrates；3) reducing the temperature of described reaction chamber, the carbon dissolved in described metallic substrates separates out and forms Graphene, so far, i.e. obtains two-dimensional layer hetero-junctions based on Graphene.Preparation method of the present invention utilizes the two-dimensional material such as transition metal substrate surface Direct precipitation boron nitride, molybdenum bisuphide, controls the thickness of low temperature institute indigenous graphite alkene further with metal Carbon Solubility difference at different temperatures.Preparation method of the present invention improves growth efficiency, reduces production cost, and decreases the impurity introduced in preparation process.
Description
Technical field
The present invention relates to the preparation method of a kind of two-dimensional layer hetero-junctions, be specifically related to a kind of two-dimensional layer based on Graphene
The preparation method of shape hetero-junctions.
Background technology
From grapheme material in 2004 with the tow-dimensions atom structure of its uniqueness, excellent physicochemical characteristics, theoretical and
Applied research all causes and unprecedented grinds the upsurge that makes internal disorder or usurp.The research of Graphene also opens the gate of two-dimensional material, causes
People have the great interest of the two-dimensional layer nano material of analog structure to other and Graphene.Up to the present, existing
Hundreds of two-dimensional material is found by people, including hexagonal boron nitride, black phosphorus and transient metal sulfide and oxide material etc..
Wherein monolayer hexagonal boron nitride has the characteristics such as the broad-band gap of 5.9eV, low-k, high-termal conductivity, can be applicable to device
Dielectric layer.Transient metal chalcogenide compound with molybdenum bisuphide as representative, energy band, between 1.0～2.0eV, the most also has concurrently
Having a lot of advantages of Graphene, the field such as scene effect transistor, sensor, electricity storage is gathered around and is had broad application prospects.Enter one
Step, by two kinds of different two-dimensional material of selective stacking, can design and prepare the hetero-junction thin-film with difference in functionality.Example
As, the hetero-junctions of Graphene and hexagonal boron nitride composition can regulate graphite by regulation and control interlayer stack angle in a big way
The band gap of alkene.Using boron nitride as dielectric layer, it is remarkably improved the carrier mobility of the heterojunction semiconductors such as molybdenum bisuphide.Two
Dimension film heterojunction can open up these new diseases field and scopes further in conjunction with the excellent properties of multiple material.
But inhomogeneity two-dimensional material performance characteristics and technology of preparing are widely different, it is directly realized by successively growth difficulty the least.Great majority
Work all use two-step growth method, such as the first material prepared is transferred to suitable substrate, redeposited the second material
Material.Complex steps, and the material homogeneity prepared in this way is poor.Scale material preparation be device application premise and
Basis, needs development one-step method badly and prepares the technology of hetero-junction thin-film, it is achieved two-dimensional material LBL self assembly for this.
Summary of the invention
It is an object of the invention to provide the preparation method of a direct step of a kind of two-dimensional layer hetero-junctions based on Graphene,
Comparing with existing method, preparation method of the present invention can obtain clean heterojunction boundary, improves growth efficiency, reduces life
Produce cost.
The preparation method of two-dimensional layer hetero-junctions based on Graphene provided by the present invention, comprises the steps:
1) it is passed through hydrogen and carbon source gas by being placed with in the reaction chamber of metallic substrates, and heats described reaction chamber and make carbon dissolution
In described metallic substrates；
2) stop being passed through described carbon source gas in described reaction chamber, keep being passed through described hydrogen, and reacting by heating source makes it
Described metallic substrates grows；
3) keeping being passed through described hydrogen, reduce the temperature of described reaction chamber, the carbon dissolved in described metallic substrates separates out shape
Become Graphene, so far, i.e. obtain two-dimensional layer hetero-junctions based on Graphene.
In above-mentioned preparation method, described reaction source is put in described reaction chamber with described substrate etc. before heating.
In above-mentioned preparation method, described metallic substrates can be at the bottom of platino, nickel substrate, corronil substrate, at the bottom of palladio, ferrum
Transition metal simple substance and the alloys thereof such as substrate, i.e. have the metal of certain Carbon Solubility.
In above-mentioned preparation method, described preparation method is carried out in CVD system, and described metallic substrates is placed in described CVD
The thermal treatment zone of system；
Described reaction source is placed in quartz boat and is positioned at the inlet end of described CVD system, described quartz boat be placed in described instead
Answer in chamber；
Step 1) before, described method includes the step that described reaction chamber carries out evacuation, when in described reaction chamber
After vacuum reaches certain stationary value, start reaction chamber is heated, and be passed through H2, it is therefore an objective to remove metal substrate surface residual
Organic substance or oxide.
In above-mentioned preparation method, step 1) before, described method also includes described metallic substrates 1000～1100
Make annealing treatment the step of 10～30min at DEG C, as carried out, at 1100 DEG C, the 30min that anneals, its objective is to make metal recrystallization, surface
More smooth, and the Organic substance of metal substrate surface can be removed further.
In above-mentioned preparation method, step 1) in, heat the temperature of described reaction chamber to 700～1400 DEG C, actual temp
Can be adjusted according to the fusing point of described metallic substrates, during as used Pt sheet or Cu-Ni alloy, heat the temperature of described reaction chamber
To 1100 DEG C.
In above-mentioned preparation method, step 1) in, described carbon source gas can be the Hydrocarbon gas such as methane, ethylene, acetylene
Body；
The speed being passed through described hydrogen can be 0～1000sccm, concretely 10sccm；
The speed being passed through described carbon source gas is 0～500sccm, concretely 5sccm or 10sccm.
In above-mentioned preparation method, step 2) in, the temperature of described growth can be 65～200 DEG C, the time of described growth
Can be 0～60min, as grown 30min at 100 DEG C.
In above-mentioned preparation method, step 2) in, described reaction source can be following 1)-5) in any one:
1) ammonia borine (NH3·BH3, Solid Source)；
2) borazine (B3H6N3, gas)；
3) diborane (B2H6, gas) and ammonia；
4) molybdenum trioxide and sulfur；
5) Tungstic anhydride. and sulfur；
Graphene/boron nitride hetero-junctions is obtained when ammonia borine, borazine or diborane and ammonia, as adopted as described in use
Graphene/molybdenum bisuphide hetero-junctions is obtained, as used Tungstic anhydride. and sulfur to obtain Graphene/bis-sulfur during with sulfur powder and molybdenum trioxide
Change tungsten hetero-junctions.
In above-mentioned preparation method, step 3) in, the temperature reducing described reaction chamber uses the cooling with 5～26 DEG C/min
Speed is down to the mode of 600～900 DEG C；
The thickness of formed Graphene can be controlled by controlling rate of temperature fall；According to the metallic substrates used not
With, the condition of above-mentioned cooling is different, and when using platinized platinum, being cooled to 600 DEG C with the rate of temperature fall of 21.6 DEG C/min can
Indigenous graphite alkene, when using Cu-Ni alloy, being cooled to 900 DEG C with the rate of temperature fall of 26 DEG C/min could indigenous graphite alkene.
In above-mentioned preparation method, described method also includes being transferred to described two-dimensional layer hetero-junctions based on Graphene
Step on substrate；
Bubbling transfer method or polystyrene transfer method is used to shift；
Described bubbling transfer method can be carried out in accordance with the following steps: growth has the metallic substrates of hetero-junctions based on Graphene
Spin coating PMMA glue, uses bubbling transfer method to be transferred on substrate, with acetone bubble except the PMMA glue of sample surfaces.
Described polystyrene transfer method can be carried out in accordance with the following steps: growth has the metal of hetero-junctions based on Graphene
Substrate spin coating polystyrene solution, dries to put into and is heated to 90 DEG C in 2molNaOH solution, Graphene/boron nitride/polystyrene
Layer will swim in NaOH solution, fish for sample, polystyrene layer and substrate attaching with substrate, the post-heating 10min temperature dried
Degree is 120 DEG C, then sample is put into the polystyrene removing residual in acetone soln.
In above-mentioned preparation method, step 1) before, described method also includes utilizing acetone, ethanol and deionized water ultrasonic
Clean the step of described metallic substrates, to remove impurity and the Organic substance on surface.
Preparation method of the present invention utilizes the two-dimensional material such as transition metal substrate surface Direct precipitation boron nitride, molybdenum bisuphide,
The thickness of low temperature institute indigenous graphite alkene is controlled further with metal Carbon Solubility difference at different temperatures.I.e. temperature is more
High metal is the biggest to the dissolubility of carbon, so at high temperature carrying out carbon dissolution, and the carbon supersaturation in metallic object when temperature reduces,
Metal surface separates out and forms Graphene.Ultimately form two-dimensional hetero-junction thin film based on Graphene.Preparation method of the present invention carries
High growth efficiency, reduces production cost, and decreases the impurity introduced in preparation process.
Accompanying drawing explanation
Fig. 1 is the CVD growth schematic diagram of preparation method of the present invention.
Fig. 2 is the growing principle figure of preparation method of the present invention.
Fig. 3 is that the subband structures boron nitride/full single-layer graphene obtained at Pt sheet at 1100 DEG C in the embodiment of the present invention 1 is heterogeneous
The SEM figure of knot.
Fig. 4 is to obtain subband structures boron nitride/full single-layer graphene hetero-junctions at Pt sheet at 1100 DEG C in the embodiment of the present invention 1
XPS spectrum (B1s).
Fig. 5 is to obtain subband structures boron nitride/full single-layer graphene hetero-junctions at Pt sheet at 1100 DEG C in the embodiment of the present invention 1
XPS spectrum (N1s).
Fig. 6 is to obtain subband structures boron nitride/full single-layer graphene hetero-junctions at Pt sheet at 1100 DEG C in the embodiment of the present invention 1
XPS spectrum (C1s).
Fig. 7 is that the AES that boron nitride/Graphene hetero-junctions prepared by the embodiment of the present invention 1 is transferred on silicon chip composes entirely.
Fig. 8 is the AES that boron nitride/Graphene hetero-junctions prepared by the embodiment of the present invention 1 transfers to the BN region on silicon chip
Depth analysis curve.
Fig. 9 is the hetero-junctions region that boron nitride/Graphene hetero-junctions prepared by the embodiment of the present invention 1 is transferred on silicon chip
AES depth analysis curve.
Figure 10 is to obtain the SEM that boron nitride/Graphene is heterogeneous in the embodiment of the present invention 2 at 1050 DEG C on Cu-Ni alloy
Figure.
Figure 11 is to obtain on Cu-Ni alloy at 1050 DEG C in the embodiment of the present invention 2 that boron nitride/Graphene is heterogeneous transfers to
Optical picture on silicon chip.
Figure 12 is to obtain on Cu-Ni alloy at 1050 DEG C in the embodiment of the present invention 2 that boron nitride/Graphene is heterogeneous transfers to
Raman spectral peak figure on silicon chip.
Detailed description of the invention
Experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, the most commercially obtain.
Embodiment 1, on Pt sheet, prepare Graphene/boron nitride hetero-junctions
The inventive method prepares the CVD growth schematic diagram of Graphene/boron nitride hetero-junctions and growing principle figure respectively such as Fig. 1
Shown in Fig. 2.
The preparation of substrate:
The Pt sheet of shearing suitable dimension, as substrate, uses acetone, ethanol and deionized water to carry out ultrasonic cleaning successively, goes
Impurity and Organic substance except surface.
The preparation of Graphene/boron nitride hetero-junctions:
First, the ammonia borine weighing 3mg is positioned in the U-shaped quartz boat remained silent in one end；By ready Pt sheet (3cm ×
3cm) putting in CVD quartz ampoule with ammonia borine reaction source, the position of Pt sheet is the centre of the thermal treatment zone, and the position in ammonia borine source is being entered
Gas end distance Pt sheet 35cm；Secondly, quartz ampoule being carried out evacuation, vacuum is evacuated to 2.26 × 10-3Torr, adds body of heater
Heat, is warming up to 1100 DEG C, is passed through 10sccm H2, and before growth, be maintained at 1100 DEG C and Pt substrate is carried out 30min's
Annealing.Finally, after 30min annealing, it is passed through the CH of 10sccm4(i.e. H2: CH4=10sccm:10sccm), it is provided that carbon source.
After 30min, turn off CH4Gas, is passed through 20sccmH2, and open the heating tape at ammonia borine reaction source is heated, temperature
Being 100 DEG C, the growth time of boron nitride is 30min.After 30min, turn off heating and the heating tape of CVD, keep 10sccmH2,
Slowly it is cooled to 600 DEG C with the cooling rate of 21.6 DEG C/min and separates out carbon acquisition Graphene, raise bell the most again and carry out quickly
Cooling, i.e. obtains Graphene/boron nitride hetero-junctions on Pt sheet.
The transfer of Graphene/boron nitride hetero-junctions:
The Graphene prepared by the present embodiment/boron nitride hetero-junctions is transferred on silicon chip: growth has Graphene/boron nitride
The Pt sheet bubbling transfer method of hetero-junctions, first spin coating PMMA glue on sample, dries, and inserts 1molNaOH solution as negative electrode
Electrolyte, anode with pure Pt sheet, electric current control～1A, the Graphene/boron nitride/PMMA glue hetero-junctions that will come off on Pt sheet
Cross three times deionized waters, remove and remain in the NaOH solution on sample, fish for sample with substrate, after drying, sample is put into third
The PMMA glue of sample surfaces is removed in ketone solution.
The SEM figure of Graphene prepared by the present embodiment/boron nitride hetero-junctions is as it is shown on figure 3, by this figure it can be seen that uniformly
Full single-layer graphene, have the boron nitride of white subband structures triangular shape above.
The XPS spectrum (B1s) of Graphene prepared by the present embodiment/boron nitride hetero-junctions as shown in Figure 4, can be seen by this figure
Go out, the peak position of B1s～190.49eV, meet the standard value of boron nitride XPS.
The XPS spectrum (N1s) of Graphene prepared by the present embodiment/boron nitride hetero-junctions is as it is shown in figure 5, can be seen by this figure
Go out, the peak position of N1s～397.8eV, meet the standard value of boron nitride XPS.
The XPS spectrum (C1s) of Graphene prepared by the present embodiment/boron nitride hetero-junctions as shown in Figure 6, can be seen by this figure
Go out, the peak position of C1s～284.38eV, meet the C-C bonding energy of Graphene.
The AES that Graphene prepared by the present embodiment/boron nitride hetero-junctions is transferred on silicon chip composes as it is shown in fig. 7, by this entirely
Figure is it can be seen that all there are the elements such as boron, nitrogen, carbon, silicon, heterojunction regions in boron nitride region and Graphene/boron nitride hetero-junctions region
The carbon element content in territory substantially many than boron nitride region, illustrate the existence of Graphene.
The AES depth analysis that Graphene prepared by the present embodiment/boron nitride hetero-junctions transfers to the BN region on silicon chip is bent
Line as shown in Figure 8, by this figure it can be seen that boron nitride region boron element and nitrogen element increase along with sputtering time, constituent content
Gradually decrease；And the content of carbon quickly reduces, illustrate that these carbons are sample surfaces absorption.
Graphene prepared by the present embodiment/boron nitride hetero-junctions is transferred to the AES degree of depth in the hetero-junctions region on silicon chip and is divided
Analysis curve is as it is shown in figure 9, by this figure it can be seen that along with sputtering, boron, nitrogen element content start to reduce, and carbon exists
There is a process increased at the beginning, illustrate that boron nitride, on Graphene, should demonstrate,prove our growth mechanism.During with sputtering
Between increase, carbon also begins to slowly reduce until silicon content increases to stable, it may be said that the hetero-junctions on bright surface by
Sputter.AES sputtering condition be 0.1min sputter depth be 0.1nm, by the AES depth analysis pair with Fig. 8 boron nitride region
Ratio, it can be seen that about～2.3nm, the thickness of boron nitride is about～1.7nm is (by the finally stabilised song of element silicon for hetero-junctions thickness
Line judges).Characterized by SEM, AES, XPS of above series of etc., it may be determined that present invention obtains matter measured vertically
Structure hetero-junction thin-film.Thus, also the explanation present invention grows preparation method simply, improves growth efficiency；Metallic substrates can weigh
Multiple use, reduces production cost；And it is a step direct growth, decreases other impurity introduced in preparation process.
Embodiment 2, on Cu-Ni alloy, prepare Graphene/boron nitride hetero-junctions
Because the Carbon Solubility of Cu-Ni alloy and Pt is different, preparation parameter is adjusted, mainly adjusts methane
Flow and temperature-fall period.
According to the preparation method in embodiment 1, use same preparation process, simply during carbon dissolution, CH4: H2Ratio
For 5sccm:10sccm；In addition, last analysis carbon step, it is down to 900 DEG C of fast coolings more slowly with the speed of 26 DEG C/min.
The SEM of Graphene prepared by the present embodiment/boron nitride hetero-junctions schemes as shown in Figure 10, by this figure it can be seen that Asia
Single-layer silicon nitride boron (dark tetragon) and single-layer graphene.
The optical picture of Graphene prepared by the present embodiment/boron nitride hetero-junctions as shown in figure 11, by this figure it can be seen that full
The boron nitride of light tetragon is had above the Graphene of monolayer.
The Raman spectral peak of Graphene prepared by the present embodiment/boron nitride hetero-junctions as shown in figure 12, can be seen by this figure
Going out, the Raman peaks in the region of hetero-junctions region and pure Graphene is had any different, and heterogeneous has a 1360cm-1The peak of boron nitride, and
The 1354cm that pure Graphene region only one of which is the faintest-1Defect peak.
Claims (10)
1. a preparation method for two-dimensional layer hetero-junctions based on Graphene, comprises the steps:
1) it is passed through hydrogen and carbon source gas by being placed with in the reaction chamber of metallic substrates, and heats described reaction chamber and make carbon dissolution in institute
State in metallic substrates；
2) stop in described reaction chamber, be passed through described carbon source gas, and reacting by heating source makes it give birth in described metallic substrates
Long；
3) reducing the temperature of described reaction chamber, the carbon dissolved in described metallic substrates separates out and forms Graphene, so far, i.e. obtains base
Two-dimensional layer hetero-junctions in Graphene.
Preparation method the most according to claim 1, it is characterised in that: described metallic substrates is at the bottom of platino, nickel substrate, copper nickel
At the bottom of alloy substrates, palladio or at the bottom of iron-based.
Preparation method the most according to claim 1 and 2, it is characterised in that: described preparation method is carried out in CVD system；
Described reaction source is placed in quartz boat and is positioned at the inlet end of described CVD system；
Step 1) before, described method includes the step that described reaction chamber carries out evacuation.
4. according to the preparation method according to any one of claim 1-3, it is characterised in that: step 1) before, described method is also
Including the step that described metallic substrates is made annealing treatment at 1000～1100 DEG C 10～30min；
Step 1) in, heat the temperature of described reaction chamber to 700～1400 DEG C.
5. according to the preparation method according to any one of claim 1-4, it is characterised in that: step 1) in, described carbon source gas is
Hydrocarbon gas；
The speed being passed through described hydrogen is 0～1000sccm, but is not zero；
The speed being passed through described carbon source gas is 0～500sccm, but is not zero.
6. according to the preparation method according to any one of claim 1-5, it is characterised in that: step 2) in, the temperature of described growth
Degree can be 65～200 DEG C, and the time of described growth can be 0～60min, but is not zero.
7. according to the preparation method according to any one of claim 1-6, it is characterised in that: step 2) in, described reaction source is
Following 1) in-5) any one:
1) ammonia borine；
2) borazine；
3) diborane and ammonia；
4) molybdenum trioxide and sulfur；
5) Tungstic anhydride. and sulfur.
8. according to the preparation method according to any one of claim 1-7, it is characterised in that: step 3) in, reduce described reaction
The temperature in chamber uses in the way of the rate of temperature fall of 5～26 DEG C/min is down to 600～900 DEG C.
9. according to the preparation method according to any one of claim 1-8, it is characterised in that: described method also includes described base
In the step that the two-dimensional layer hetero-junctions of Graphene is transferred on substrate；
Bubbling transfer method or polystyrene transfer method is used to shift.
10. according to the preparation method according to any one of claim 1-9, it is characterised in that: step 1) before, described method is also
Including utilizing the step of metallic substrates described in acetone, ethanol and deionized water ultrasonic cleaning.
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| CN109019569B (en) * | 2017-06-08 | 2021-05-28 | 中国科学院金属研究所 | High-quality graphene/two-dimensional metal carbide crystal vertical heterostructure material and preparation method thereof |
| CN108923257A (en) * | 2018-06-13 | 2018-11-30 | 东南大学 | A kind of laser diode and preparation method thereof |
| CN109767992A (en) * | 2019-01-16 | 2019-05-17 | 深圳天元羲王材料科技有限公司 | Radiator heat-dissipation layer preparation method and radiator |
| CN112110440A (en) * | 2019-06-19 | 2020-12-22 | 中国科学院金属研究所 | Preparation method of high-quality uniform multilayer graphene film with specific stacking mode |
| CN110954570A (en) * | 2019-11-11 | 2020-04-03 | 华东师范大学 | Method for stripping two-dimensional material grown on sapphire substrate by temperature control bubbling |
| CN110954570B (en) * | 2019-11-11 | 2020-08-04 | 华东师范大学 | Method for stripping two-dimensional material grown on sapphire substrate by temperature control bubbling |
| CN111637801A (en) * | 2020-05-21 | 2020-09-08 | 西安交通大学 | PMMA-based graphene burst pressure test sensor and manufacturing method thereof |
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