CN105668555B - A kind of method for preparing three-dimensional grapheme - Google Patents
A kind of method for preparing three-dimensional grapheme Download PDFInfo
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- CN105668555B CN105668555B CN201610008722.0A CN201610008722A CN105668555B CN 105668555 B CN105668555 B CN 105668555B CN 201610008722 A CN201610008722 A CN 201610008722A CN 105668555 B CN105668555 B CN 105668555B
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- C01—INORGANIC CHEMISTRY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of method for preparing three-dimensional grapheme.This method, be during chemical vapor deposition, using without method of the template without catalyst directly by controlling carbon source flow in a variety of Grown three-dimensional graphemes.Carbon source concentration is controlled so as to reach to three-dimensional grapheme density and highly controllable effect by changing the flow of carbon source.Method disclosed by the invention, compared with traditional method, the cumbersome and cost of preparation process is greatly reduced, and improve the controllability to prepared three-dimensional grapheme density and height.
Description
Technical field
The invention belongs to Material Field, is related to a kind of method for preparing three-dimensional grapheme.
Background technology
Graphene is a kind of carbon material of monoatomic layer thickness, has a series of unique properties, such as extraordinary current-carrying
Transport factor (200,000cm2V-1s-1), thermal conductivity (the 5300W m of superelevation-1K-1), fabulous light transmission rate (97.7%) and
Excellent mechanical performance.In recent years, graphene has been reported in the crowds such as photoelectronics, energy conversion, electro-catalysis, biological detection
It is multi-field that there is potential application.Thus, in order to realize these applications, to the size of graphene, pattern, marginal texture, functionalization
Regulate and control the property of graphene etc. substantial amounts of research has been carried out.Up to the present, two-dimentional intrinsic graphene has been extended to
The graphene network structure of the graphene quantum dot of zero dimension, one-dimensional graphene nanobelt and three-dimensional.Wherein, three-dimensional grapheme
Due to its unique morphological structure, it is proved to many electricity, chemistry and machines for being different from two-dimensional graphene body
Tool property.Due to very high specific surface area and highdensity avtive spot, three-dimensional grapheme be widely used in biology with
Chemical detection (ACS Appl.Mater.Inter.2012,4,3129.；Small2013,9,1703.；Nanoscale2015,7,
2427.).Excellent electrical conductivity and the surface area of superelevation allow three-dimensional grapheme as application of electrode in high performance flexibility
Ultracapacitor (Small2011,7,3163.；ACS Nano2012,6,3206.；ACS Nano2013,7,4042.).Due to
The charge transport ability of its unique vertical profile, high marginal density and protrusion, three-dimensional grapheme are proved to have excellent
Field emission performance (Appl.Phy.Lett.2011,98,263104.).In addition, as due to low-density, adjustable
The compressibility of electrical conductivity and superelevation, three-dimensional grapheme are used for ultralight, controllable high performance wideband microwave absorption
(Adv.Mater.2015,27,2049.).Ground it is thereby achieved that prepared by gentle, controllable, efficient three-dimensional grapheme for science
Study carefully and commercial Application all has great importance.
Three-dimensional grapheme includes two kinds of forms of grapheme foam and vertical stand-up graphene.Wherein grapheme foam is substantially
Prepared using template, for example grown using chemical vapour deposition technique in the templates such as three-dimensional metal foam, carbon network structure
Obtain the grapheme foam (Nat.Mater.2011,10,424. of three-dimensional；ACS Nano2012,6,4020.；
Angew.Chem.Int.Ed.2014,53,1404.；Adv.Mater.2015,27,2049.).But such a method needs complexity
Stencil design and follow-up template etching remove template.And template and the residual of etching agent are typically inevitable
, often influence even to reduce the performance of final three-dimensional grapheme.And vertical stand-up graphene be typically all by wait from
Daughter assistant chemical vapor deposition or Microwave Irradiation Assisted Chemical are vapor-deposited to prepare (Adv.Mater.2002,14,64.；
Adv.Energy Mater.2013,3,1316.；Adv.Mater.2013,25,5799.；Adv.Mater.2013,25,
5638.；ACS Nano2014,8,5873.).But these methods need to use extra equipment and harsh growing environment
Such as ultralow pressure；And the pattern of prepared three-dimensional grapheme, density, height etc. be difficult to it is controllable.If can be more
The controllable high-efficiency growth of three-dimensional grapheme is directly realized by kind substrate, for the large area preparation of three-dimensional grapheme and extensive work
Industry, which is applied, to open up new road.
The content of the invention
It is an object of the invention to provide a kind of method for preparing three-dimensional grapheme.
The method provided by the invention for preparing three-dimensional grapheme, comprises the following steps：
In hydrogen and argon gas atmosphere, be passed through carbon-source gas in carrying out chemical vapor deposition on substrate, deposition finish after
The three-dimensional grapheme is obtained on the substrate.
In above-mentioned preparation method, the substrate is monocrystalline silicon, silica/silicon, quartz plate or zirconium dioxide/silicon；
The thickness of the monocrystalline silicon is 250-500 microns, specially 400 microns；
In the silica/silicon, the thickness of silicon dioxide layer is 250-400 nanometers, specially 300 nanometers；Silicon layer
Thickness is 250-500 microns, specially 400 microns；
The thickness of the quartz plate is 1-3 millimeters, specially 1 millimeter；
In the zirconium dioxide/silicon, the thickness of titanium dioxide zirconium layer is 10-50 nanometers, specially 20 nanometers；The thickness of silicon layer
For 250-500 microns, specially 400 microns.
The carbon-source gas are methane, ethene or ethane, specially methane；
The flow-rate ratio of the carbon-source gas, hydrogen and argon gas is 7.0：50：50 to 14.0：50：50；
Specifically, the flow of the carbon source is 7.0-14.0sccm, concretely 7.0,7.5,8.0,8.5,9.0,9.5,
10.0th, 10.5,11.0,11.5,12.0,12.5,13.0,13.5 or 14.0sccm；
The flow of the hydrogen is 50sccm；
The flow of the argon gas is 50sccm.
The flow-rate ratio of the carbon source, hydrogen and argon gas is 7.0-10.0：50：When 50, the density of gained three-dimensional grapheme with
Height is smaller；When the flow of the carbon source is specially 7.0 or 7.5 or 8.0 or 8.5 or 9.0 or 9.5 or 10.0sccm, the hydrogen
The flow of gas is 50sccm, and the flow of the argon gas is 50sccm；
The flow-rate ratio of the carbon source, hydrogen and argon gas is 10.0-14.0：50：When 50, the density of gained three-dimensional grapheme with
It is highly larger；Wherein, the flow of the carbon source be specially 10.5 or 11.0 or 11.5 or 12.0 or 12.5 or 13.0 or 13.5 or
During 14.0sccm, the flow of the hydrogen is 50sccm, and the flow of the argon gas is 50sccm；
In the chemical vapor deposition step, the time is 2-8 hours, specially 2,4 or 6 hours；
Pressure is 0-1.01 × 105Pa, but be not 0, the pressure is specially 1.01 × 105Pa。
Temperature is 1000-1250 DEG C, specially 1130 DEG C.
Methods described also comprises the following steps：
Before the chemical vapor deposition step, the substrate is annealed.
Specifically, in the annealing steps, the atmosphere of annealing is hydrogen and argon gas atmosphere；
The flow of hydrogen is 10-100sccm, specially 50sccm；
The flow of argon gas is 10-100sccm, specially 50sccm；
The time of annealing is 10-60 minutes, specially 30 minutes.
In addition, methods described also comprises the following steps：
Before the chemical vapor deposition step, the substrate is pre-processed as follows：The substrate is used successively
After deionized water, acetone, EtOH Sonicate cleaning, nitrogen drying, then with the mixed liquid dipping being made up of the concentrated sulfuric acid and hydrogen peroxide, go
Ionized water is cleaned by ultrasonic, nitrogen drying；
Wherein, in the mixed liquor being made up of the concentrated sulfuric acid and hydrogen peroxide, the mass percentage concentration of hydrogen peroxide is 70%；Institute
The volume ratio for stating the concentrated sulfuric acid and hydrogen peroxide is 3：7；
In the soaking step, the concretely 30 minutes time of immersion；
In the ultrasonic cleaning step, concretely 3 minutes time.
Methods described may also include the steps of：After the chemical vapor deposition step, by system in argon gas and hydrogen
Cooled down in the mixed atmosphere of gas；In the cooling step, the flow of argon gas is specially 50sccm；The flow of hydrogen is specially
50sccm；
In addition, the three-dimensional grapheme being prepared according to the method described above, falls within protection scope of the present invention.Wherein, institute
The density and height for stating three-dimensional grapheme can be with accuracy controllings.
The method provided by the invention for preparing three-dimensional grapheme, it is during chemical vapor deposition, using without template
Method without catalyst is directly by controlling carbon source flow in a variety of Grown three-dimensional graphemes.By the stream for changing carbon source
Measure to control carbon source concentration so as to reach density and highly controllable effect.This method has feature and advantage：
1. of the invention disclose the method that three-dimensional grapheme is grown in thermal chemical vapor deposition system for the first time.
2. of the invention disclose the deciding factor that carbon source flow is the graphene dimension for influenceing growth for the first time.
3. of the invention disclose the mechanism that three-dimensional grapheme grows in thermal chemical vapor deposition system for the first time.
4. the method for the invention disclosed for the first time to three-dimensional grapheme density and height Effective Regulation.
5. of the invention disclose growth of the three-dimensional grapheme on a variety of substrates for the first time.
6. method disclosed by the invention, compared with traditional method, template that both need not be complicated is also without extra
A kind of plasma apparatus, there is provided method of with can realizing more efficient milder growing three-dimensional structure graphite alkene.
Brief description of the drawings
Fig. 1 is the low power and high power electron scanning micrograph of the three-dimensional grapheme of low-density prepared by embodiment 1；
Fig. 2 is 45 degree of dip scanning electron micrographs of the three-dimensional grapheme of low-density prepared by embodiment 1；
Fig. 3 is the low power and high power transmission electron microscope figure of the three-dimensional grapheme of low-density prepared by embodiment 1；
Fig. 4 is the low power and high power electron scanning micrograph of highdensity three-dimensional grapheme prepared by embodiment 2；
Fig. 5 is the low power and high power transmission electron microscope figure of highdensity three-dimensional grapheme prepared by embodiment 2；
Fig. 6 is the graphite Raman spectrogram that highdensity three-dimensional grapheme prepared by embodiment 2 has typical representative；
Fig. 7 is the AFM graphics of the three-dimensional grapheme of different height prepared by control growth conditions；
Fig. 8 is scanning electron microscope diagram of the three-dimensional grapheme with the growth change process of time.
Fig. 9 is the electron scanning micrograph of planar graphene prepared by reference examples 1；
Figure 10 is the Raman spectrogram of planar graphene prepared by reference examples 1；
Figure 11 is the electron scanning micrograph of amorphous carbon prepared by reference examples 2；
Figure 12 is the Raman spectrogram of amorphous carbon prepared by reference examples 2；
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
It is conventional method unless otherwise instructed to state method.The raw material can obtain from open commercial sources unless otherwise instructed.
The three-dimensional grapheme of embodiment 1, thermal chemical vapor deposition method direct growth low-density
1) silicon growth substrate is cleaned：
Silicon is respectively cleaned by ultrasonic 3 minutes with deionized water, acetone, ethanol successively, nitrogen drying, with 3:7 concentrated sulfuric acid/
70% hydrogen peroxide dipping 30 minutes, then be cleaned by ultrasonic 3 minutes with deionized water, nitrogen drying；
2) substrate (400 microns of thick silicon) by cleaning is positioned in quartz ampoule.Quartz ampoule is put into tube furnace again, silicon
Substrate is directed at the probe zone of tube furnace, is passed through 50sccm hydrogen and after 20 minutes, begins to warm up with 50sccm argon gas, work as tube furnace
When the temperature of central area reaches 1130 DEG C, stabilizing annealing 30 minutes is kept；
3) graphene is grown：
It is 1130 DEG C to maintain the temperature in step 2) in tubular type hearthstone English pipe, be passed through methane that flow is 8sccm and
50sccm hydrogen and 50sccm argon gas, 1.01 × 105After being grown 4 hours under Pa pressure, methane is closed, is in flow
Room temperature is cooled to tube furnace under 50sccm hydrogen and 50sccm argon gas mixed airflows, obtains low-density three provided by the invention
Graphene is tieed up, as shown in Fig. 1 and Fig. 2 electron scanning micrographs, and sample is prepared and is characterized through transmission electron microscope, such as
Shown in Fig. 3.
As seen from the figure, the graphene prepared by the embodiment has the three-dimensional appearance perpendicular to substrate, and vertical stand-up
Graphene film density ratio it is relatively low.
Embodiment 2, the highdensity three-dimensional grapheme of thermal chemical vapor deposition method direct growth
According to 1 identical method of embodiment, only methane flow will be passed through in step 3) increases to 12sccm.Pass through
Increase the flow of methane so as to change the concentration of carbon atom, and then influence the density of gained three-dimensional grapheme, Fig. 4 is the height obtained
The three-dimensional grapheme low power and high power scanning electron microscope diagram of density.And sample is prepared to characterize through transmission electron microscope,
As shown in Figure 5.And Raman sign is carried out to highdensity three-dimensional grapheme, as shown in Figure 6.
As seen from the figure, with the increase of methane flow, the preparation-obtained upright graphene film of three-dimensional perpendicular on substrate
Density increases.
The three-dimensional grapheme of embodiment 3, thermal chemical vapor deposition method direct growth different height
According to 1 identical method of embodiment, will be only passed through in step 3) methane flow difference value 9,11,
13sccm.The differentiation of three-dimensional grapheme density as obtained by observation, it is found that the height of gained three-dimensional grapheme changes from low to high,
As shown in atomic force microscopy diagram 7.
As seen from the figure, with the increase of methane flow, the preparation-obtained upright graphene film of three-dimensional perpendicular on substrate
Height gradually increase.
The change procedure of embodiment 4, thermal chemical vapor deposition method direct growth three-dimensional grapheme
According to 1 identical method of embodiment, only by step 3) growth time distinguish value 2,4,6 hours, see
The change procedure of gained graphene pattern is examined, it is found that gained three-dimensional grapheme first just obtains after graphene film grows connection film forming
The graphene of three-dimensional structure, it is illustrated in figure 8 corresponding to the different graphenes in 3 stages obtained by 3 values of growth time and sweeps
Retouch electron microscope picture.
As seen from the figure, graphene prolong first substrate planar growth, connect film forming after regrowth just obtain perpendicular to base
The three-dimensional grapheme at bottom.
Reference examples 1, thermal chemical vapor deposition method growth two-dimensional graphene according to 1 identical method of embodiment, only
6sccm is reduced to by methane flow is passed through in step 3).Change the concentration of carbon atom by reducing the flow of methane, and then
The structure and pattern of material prepared by influence, Fig. 9 are the planar graphene obtained under conditions of less than 7sccm methane
Scanning electron microscope diagram.And Raman sign is carried out to preparing sample, as shown in Figure 10.As seen from the figure, in other specification
In the case of constant, the plane graphene of two dimension is can only obtain when methane flow is less than 7sccm.
Reference examples 2, thermal chemical vapor deposition method growth amorphous carbon
According to 1 identical method of embodiment, only methane flow will be passed through in step 3) and brings up to 15sccm.Pass through
Increase the flow of methane so as to change the concentration of carbon atom, and then the structure and pattern of material prepared by influence, Figure 11 is this
The scanning electron microscope diagram of the amorphous carbon obtained under part.And Raman sign is carried out to preparing sample, as shown in figure 12.
As seen from the figure, in the case where other specification is constant, can only obtain when methane flow is higher than 14sccm amorphous
Carbon.
Claims (7)
1. a kind of method for preparing three-dimensional grapheme, comprises the following steps：
In hydrogen and argon gas atmosphere, carbon-source gas are passed through in carrying out chemical vapor deposition on substrate, deposits and finishes after described
The three-dimensional grapheme is obtained on substrate；
The flow-rate ratio of the carbon-source gas, hydrogen and argon gas is 7.0：50：50 to 14.0：50：50；
In the chemical vapor deposition step, temperature is 1000-1250 DEG C.
2. according to the method for claim 1, it is characterised in that：The substrate is monocrystalline silicon, silica/silicon, quartz plate
Or zirconium dioxide/silicon；
The thickness of the monocrystalline silicon is 250-500 microns；
In the silica/silicon, the thickness of silicon dioxide layer is 250-400 nanometers；The thickness of silicon layer is 250-500 microns；
The thickness of the quartz plate is 1-3 millimeters；
In the zirconium dioxide/silicon, the thickness of titanium dioxide zirconium layer is 10-50 nanometers；The thickness of silicon layer is 250-500 microns.
3. method according to claim 1 or 2, it is characterised in that：The carbon-source gas are methane, ethene or ethane；
The flow of the carbon source is 7.0-14.0sccm；
The flow of the hydrogen is 50sccm；
The flow of the argon gas is 50sccm.
4. method according to claim 1 or 2, it is characterised in that：In the chemical vapor deposition step, time 2-8
Hour；
Pressure is 0-1.01 × 105Pa, but be not 0.
5. method according to claim 1 or 2, it is characterised in that：Methods described also comprises the following steps：
Before the chemical vapor deposition step, the substrate is annealed.
6. according to the method for claim 5, it is characterised in that：In the annealing steps, the atmosphere of annealing is hydrogen and argon
Gas atmosphere；
The flow of hydrogen is 10-100sccm；
The flow of argon gas is 10-100sccm；
The time of annealing is 10-60 minutes.
7. the three-dimensional grapheme that any methods described is prepared in claim 1-6.
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| CN106324291B (en) * | 2016-08-15 | 2018-10-30 | 清华大学 | For the graphene film talent scout needle of atomic force microscope and the acquisition methods of friction coefficient |
| CN106323867B (en) * | 2016-08-15 | 2019-04-05 | 清华大学 | The preparation method of graphene film ball |
| CN107452841B (en) * | 2017-09-04 | 2019-07-09 | 湘能华磊光电股份有限公司 | LED epitaxial growth method based on graphene |
| CN110354700B (en) * | 2018-04-11 | 2022-06-24 | 广州墨羲科技有限公司 | Polymer graphene composite filtering membrane, and manufacturing method and application thereof |
| CN109502575B (en) * | 2018-12-25 | 2021-09-21 | 江苏鲁汶仪器有限公司 | Method for preparing large-area graphene through chemical vapor deposition |
| CN109850908B (en) * | 2019-04-12 | 2020-01-14 | 中国科学院重庆绿色智能技术研究院 | Preparation method and product of silicon dioxide/graphene compound |
| CN110342502B (en) * | 2019-06-26 | 2021-07-20 | 上海交通大学 | Preparation method of graphene composite carbon material with graphite flake in-situ growth |
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| CN102161482A (en) * | 2011-01-25 | 2011-08-24 | 中国科学院化学研究所 | Method for preparing graphene |
| CN102874801A (en) * | 2012-10-15 | 2013-01-16 | 中国科学院上海微***与信息技术研究所 | Preparation method for graphene |
| CN104018136A (en) * | 2014-04-30 | 2014-09-03 | 中国科学院重庆绿色智能技术研究院 | Method for directly and conformally covering graphene film on full surface of substrate with three-dimensional structure |
| CN104211054A (en) * | 2014-09-09 | 2014-12-17 | 中国科学院化学研究所 | Method for controllably preparing graphene |
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| CN102161482A (en) * | 2011-01-25 | 2011-08-24 | 中国科学院化学研究所 | Method for preparing graphene |
| CN102874801A (en) * | 2012-10-15 | 2013-01-16 | 中国科学院上海微***与信息技术研究所 | Preparation method for graphene |
| CN104018136A (en) * | 2014-04-30 | 2014-09-03 | 中国科学院重庆绿色智能技术研究院 | Method for directly and conformally covering graphene film on full surface of substrate with three-dimensional structure |
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