CN105668555A - Method for preparing three-dimensional graphene - Google Patents
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a method for preparing three-dimensional graphene. According to the method, in a process of chemical vapor deposition, three-dimensional graphene is grown on a variety of substrates directly by controlling the carbon source flow quantity by means of a template-free catalyst-free method. The concentration of the carbon source is controlled by changing the flow quantity of the carbon source, so as to achieve the effect of controllable density and height of the three-dimensional graphene. Compared with a traditional method, the method disclosed by the invention greatly reduces the complexity and cost of the preparation process, and improves the controllability of the density and height of the prepared three-dimensional graphene.
Description
Technical field
The invention belongs to Material Field, relate to a kind of method preparing three-dimensional grapheme.
Background technology
Graphene is the material with carbon element of a kind of monoatomic layer thickness, has the character of a series of uniqueness, such as extraordinary carrier mobility (200,000cm2V-1s-1), the thermal conductivity (5300Wm of superelevation-1K-1), fabulous light transmission rate (97.7%) and the mechanical performance of excellence. In recent years, Graphene has been reported in the various fields such as optoelectronics, energy conversion, electro-catalysis, biological detection and has had potential application. Thus, in order to realize these application, the size of Graphene, pattern, marginal texture, functionalization etc. are carried out substantial amounts of research to regulate and control the character of Graphene. Up to the present, the intrinsic Graphene of two dimension 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 the appearance structure feature of its uniqueness, is proved to have and many is different from the electricity of two-dimensional graphene body, chemistry and engineering properties. Owing to having significantly high specific surface area and highdensity avtive spot, three-dimensional grapheme is widely used in biological and chemical detection (ACSAppl.Mater.Inter.2012,4,3129.; Small2013,9,1703.; Nanoscale2015,7,2427.). Excellent electrical conductivity and the surface area of superelevation make the three-dimensional grapheme can as application of electrode in high performance flexible super capacitor (Small2011,7,3163.; ACSNano2012,6,3206.; ACSNano2013,7,4042.). Due to the vertical profile of its uniqueness, high marginal density and prominent charge transport ability, three-dimensional grapheme is proved to the field emission performance (Appl.Phy.Lett.2011,98,263104.) with excellence. Additionally, as the compressibility owing to having low-density, adjustable electrical conductivity and superelevation, three-dimensional grapheme is used to ultralight, controlled high performance wideband microwave absorption (Adv.Mater.2015,27,2049.). It is thereby achieved that three-dimensional grapheme gentle, controlled, high efficiency preparation all has great importance for scientific research and commercial Application.
Three-dimensional grapheme includes grapheme foam and two kinds of forms of vertical stand-up Graphene. Wherein grapheme foam substantially adopts template synthesis, such as utilizes chemical vapour deposition technique growth in the templates such as three-dimensional metal foam, carbon network structure to obtain the grapheme foam (Nat.Mater.2011,10,424. of three-dimensional; ACSNano2012,6,4020.;Angew.Chem.Int.Ed.2014,53,1404.; Adv.Mater.2015,27,2049.). But this kind of method needs complicated stencil design and follow-up template etching to remove template. And the residual of template and etching agent is usually inevitably, often affects the performance even reducing final three-dimensional grapheme. And vertical stand-up Graphene is typically all and prepares (Adv.Mater.2002,14,64. by plasma auxiliary chemical vapor deposition or Microwave Irradiation Assisted Chemical vapour deposition; Adv.EnergyMater.2013,3,1316.; Adv.Mater.2013,25,5799.; Adv.Mater.2013,25,5638.; ACSNano2014,8,5873.). But these methods need to use extra equipment and harsh growing environment such as ultralow pressure etc.; And the pattern of prepared three-dimensional grapheme, density, height etc. are difficult to controlled. If able to be directly realized by the controllable high-efficiency growth of three-dimensional grapheme in multiple substrate, the large area for three-dimensional grapheme prepares and wide range of industrial applications will open up new road.
Summary of the invention
It is an object of the invention to provide a kind of method preparing three-dimensional grapheme.
The method preparing three-dimensional grapheme provided by the invention, comprises the steps:
In hydrogen and argon gas atmosphere, pass into carbon-source gas on substrate, carry out chemical vapour deposition (CVD), on described substrate, after deposition, obtain described three-dimensional grapheme.
In above-mentioned preparation method, described substrate is monocrystal silicon, silica/silicon, piezoid or zirconium dioxide/silicon;
The thickness of described monocrystal silicon is 250-500 micron, is specially 400 microns;
In described silica/silicon, the thickness of silicon dioxide layer is 250-400 nanometer, is specially 300 nanometers; The thickness of silicon layer is 250-500 micron, is specially 400 microns;
The thickness of described piezoid is 1-3 millimeter, is specially 1 millimeter;
In described zirconium dioxide/silicon, the thickness of titanium dioxide zirconium layer is 10-50 nanometer, is specially 20 nanometers; The thickness of silicon layer is 250-500 micron, is specially 400 microns.
Described carbon-source gas is methane, ethylene or ethane, is specially methane;
The flow-rate ratio of described carbon-source gas, hydrogen and argon is 7.0:50:50 to 14.0:50:50;
Concrete, the flow of described carbon source is 7.0-14.0sccm, concretely 7.0,7.5,8.0,8.5,9.0,9.5,10.0,10.5,11.0,11.5,12.0,12.5,13.0,13.5 or 14.0sccm;
The flow of described hydrogen is 50sccm;
The flow of described argon is 50sccm.
When the flow-rate ratio of described carbon source, hydrogen and argon is 7.0-10.0:50:50, the density of gained three-dimensional grapheme is with highly less; The flow of described carbon source is specially 7.0 or 7.5 or 8.0 or 8.5 or 9.0 or 9.5 or during 10.0sccm, the flow of described hydrogen is 50sccm, and the flow of described argon is 50sccm;
When the flow-rate ratio of described carbon source, hydrogen and argon is 10.0-14.0:50:50, the density of gained three-dimensional grapheme is with highly bigger; Wherein, the flow of described carbon source is 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 described hydrogen is 50sccm, and the flow of described argon is 50sccm;
In described chemical vapor deposition step, the time is 2-8 hour, is specially 2,4 or 6 hours;
Pressure is 0-1.01 × 105Pa, but be not 0, described pressure is specially 1.01 × 105Pa。
Temperature is 1000-1250 DEG C, is specially 1130 DEG C.
Described method also comprises the steps:
Before described chemical vapor deposition step, described substrate is annealed.
Concrete, in described annealing steps, the atmosphere of annealing is hydrogen and argon gas atmosphere;
The flow of hydrogen is 10-100sccm, is specially 50sccm;
The flow of argon is 10-100sccm, is specially 50sccm;
The time of annealing is 10-60 minute, is specially 30 minutes.
It addition, described method also comprises the steps:
Before described chemical vapor deposition step, described substrate is carried out following pretreatment: after being cleaned with deionized water, acetone, EtOH Sonicate successively by described substrate, nitrogen dries up, then with the mixed liquid dipping being made up of concentrated sulphuric acid and hydrogen peroxide, deionized water ultrasonic cleaning, nitrogen dries up;
Wherein, in the described mixed liquor being made up of concentrated sulphuric acid and hydrogen peroxide, the mass percentage concentration of hydrogen peroxide is 70%; The volume ratio of described concentrated sulphuric acid and hydrogen peroxide is 3:7;
In described soaking step, the concretely 30 minutes time of immersion;
In described ultrasonic cleaning step, concretely 3 minutes time.
Described method may also include the steps of: after described chemical vapor deposition step, system is cooled down in the mixed atmosphere of argon and hydrogen; In described cooling step, the flow of argon is specially 50sccm; The flow of hydrogen is specially 50sccm;
Additionally, the three-dimensional grapheme prepared according to the method described above, fall within protection scope of the present invention. Wherein, the density of described three-dimensional grapheme with highly can accuracy controlling.
The method preparing three-dimensional grapheme provided by the invention, is in the process of chemical vapour deposition (CVD), utilizes the method without template catalyst-free either directly through controlling carbon source flow at multiple Grown three-dimensional grapheme. Carbon source concentration is controlled thus reaching density and highly controllable effect by changing the flow of carbon source. The method has feature and advantage:
1. the present invention discloses the method growing three-dimensional grapheme in thermal chemical vapor deposition system first time.
2. the present invention discloses the deciding factor that carbon source flow is the Graphene dimension of impact growth first time.
3. the present invention discloses the mechanism of three-dimensional grapheme growth in thermal chemical vapor deposition system first time.
4. the present invention discloses the method to three-dimensional grapheme density with height Effective Regulation first time.
5. the present invention discloses three-dimensional grapheme growth on multiple substrate first time.
6. method disclosed by the invention, compared with traditional method, template that both need not be complicated is also without extra plasma apparatus, it is provided that a kind of method that can realize more efficient milder ground growing three-dimensional structure graphite alkene.
Accompanying drawing explanation
Fig. 1 is low power and the high power electron scanning micrograph of the low-density three-dimensional grapheme of embodiment 1 preparation;
Fig. 2 is 45 degree of dip scanning electron micrographs of the low-density three-dimensional grapheme of embodiment 1 preparation;
Fig. 3 is low power and the high power transmission electron microscope figure of the low-density three-dimensional grapheme of embodiment 1 preparation;
Fig. 4 is low power and the high power electron scanning micrograph of the highdensity three-dimensional grapheme of embodiment 2 preparation;
Fig. 5 is low power and the high power transmission electron microscope figure of the highdensity three-dimensional grapheme of embodiment 2 preparation;
Fig. 6 is the graphite Raman spectrogram that highdensity three-dimensional grapheme prepared by embodiment 2 has typical representative;
Fig. 7 is the atomic force microscope graphics of the three-dimensional grapheme controlling differing heights prepared by growth conditions;
Fig. 8 is the scanning electron microscope diagram of three-dimensional grapheme growth change process in time.
Fig. 9 is the electron scanning micrograph of the planar Graphene of reference examples 1 preparation;
Figure 10 is the Raman spectrogram of the planar Graphene of reference examples 1 preparation;
Figure 11 is the electron scanning micrograph of the amorphous carbon of reference examples 2 preparation;
Figure 12 is the Raman spectrogram of the amorphous carbon of reference examples 2 preparation;
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following example. Described method is conventional method if no special instructions. Described raw material if no special instructions all can from being openly either commercially available.
Embodiment 1, the low-density three-dimensional grapheme of thermal chemical vapor deposition method direct growth
1) silicon growth substrate is cleaned:
By silicon successively with deionized water, acetone, each ultrasonic cleaning of ethanol 3 minutes, nitrogen dries up, and with concentrated sulphuric acid/70% hydrogen peroxide dipping 30 minutes of 3:7, then with deionized water ultrasonic cleaning 3 minutes, nitrogen dries up;
2) clean substrate (silicon 400 microns thick) is positioned in quartz ampoule. Again quartz ampoule is put in tube furnace, the probe zone of silicon substrate alignment tube furnace, pass into 50sccm hydrogen and after 20 minutes, begin to warm up with 50sccm argon, when the temperature of tube furnace central area reaches 1130 DEG C, remain stable for annealing 30 minutes;
3) growth Graphene:
Maintain step 2) in temperature in tube furnace quartz ampoule be 1130 DEG C, pass into the hydrogen of methane that flow is 8sccm and 50sccm and the argon of 50sccm, 1.01 × 105After growing 4 hours under Pa pressure, close methane, it is cooled to room temperature with tube furnace under the hydrogen that flow is 50sccm and 50sccm argon mixed airflow, obtain low-density three-dimensional grapheme provided by the invention, as shown in Fig. 1 and Fig. 2 electron scanning micrograph, and prepare sample to characterize through transmission electron microscope, as shown in Figure 3.
As seen from the figure, the Graphene prepared by this embodiment has a perpendicular to the three-dimensional appearance of substrate, and the graphene film density ratio of vertical stand-up is relatively low.
Embodiment 2, the highdensity three-dimensional grapheme of thermal chemical vapor deposition method direct growth
According to method identical with embodiment 1, only by step 3) in pass into methane flow and increase to 12sccm. By the flow of increase methane thus changing the concentration of carbon atom, and then affecting the density of gained three-dimensional grapheme, Fig. 4 is the highdensity three-dimensional grapheme low power and high power scanning electron microscope diagram that obtain. And prepare sample to characterize through transmission electron microscope, as shown in Figure 5. And highdensity three-dimensional grapheme is carried out Raman sign, as shown in Figure 6.
As seen from the figure, along with the increase of methane flow, on substrate, the density of the upright graphene film of preparation-obtained three-dimensional perpendicular increases.
Embodiment 3, thermal chemical vapor deposition method direct growth differing heights three-dimensional grapheme
According to method identical with embodiment 1, only by step 3) in pass into methane flow respectively value 9,11,13sccm. By observing the differentiation of gained three-dimensional grapheme density, it has been found that the height of gained three-dimensional grapheme changes from low to high, as shown in atomic force microscope Fig. 7.
As seen from the figure, along with the increase of methane flow, on substrate, the height of the upright graphene film of preparation-obtained three-dimensional perpendicular is gradually increased.
Embodiment 4, thermal chemical vapor deposition method direct growth three-dimensional grapheme change procedure
According to method identical with embodiment 1, only by step 3) in growth time respectively value 2,4,6 hours, observe the change procedure of gained Graphene pattern, find that gained three-dimensional grapheme first just obtains the Graphene of three dimensional structure after graphene film growth connects film forming, be illustrated in figure 8 the scanning electron microscope diagram that the different Graphenes in 3 stages of 3 value gained of growth time are corresponding.
As seen from the figure, first Graphene prolongs the growth of substrate planar, and after connecting film forming, regrowth just obtains being perpendicular to the three-dimensional grapheme of substrate.
Reference examples 1, thermal chemical vapor deposition method growth two-dimensional graphene is according to method identical with embodiment 1, only by step 3) in pass into methane flow and be reduced to 6sccm. By reducing the flow of methane thus changing the concentration of carbon atom, and then the structure of the prepared material of impact and pattern, Fig. 9 is the scanning electron microscope diagram of the planar Graphene obtained lower than 7sccm methane when. And carry out Raman sign to preparing sample, as shown in Figure 10. As seen from the figure, when other parameter constants, can only obtain the plane Graphene of two dimension when methane flow is lower than 7sccm.
Reference examples 2, thermal chemical vapor deposition method growth amorphous carbon
According to method identical with embodiment 1, only by step 3) in pass into methane flow and bring up to 15sccm. By increasing the flow of methane thus changing the concentration of carbon atom, and then the structure of the prepared material of impact and pattern, Figure 11 is the scanning electron microscope diagram of the amorphous carbon obtained under this condition. And carry out Raman sign to preparing sample, as shown in figure 12.
As seen from the figure, when other parameter constants, can only obtain amorphous carbon when methane flow is higher than 14sccm.
Claims (7)
1. the method preparing three-dimensional grapheme, comprises the steps:
In hydrogen and argon gas atmosphere, pass into carbon-source gas on substrate, carry out chemical vapour deposition (CVD), on described substrate, after deposition, obtain described three-dimensional grapheme.
2. method according to claim 1, it is characterised in that: described substrate is monocrystal silicon, silica/silicon, piezoid or zirconium dioxide/silicon;
The thickness of described monocrystal silicon is 250-500 micron;
In described silica/silicon, the thickness of silicon dioxide layer is 250-400 nanometer; The thickness of silicon layer is 250-500 micron;
The thickness of described piezoid is 1-3 millimeter;
In described zirconium dioxide/silicon, the thickness of titanium dioxide zirconium layer is 10-50 nanometer; The thickness of silicon layer is 250-500 micron.
3. method according to claim 1 and 2, it is characterised in that: described carbon-source gas is methane, ethylene or ethane;
The flow-rate ratio of described carbon-source gas, hydrogen and argon is 7.0:50:50 to 14.0:50:50;
Concrete, the flow of described carbon source is 7.0-14.0sccm;
The flow of described hydrogen is 50sccm;
The flow of described argon is 50sccm.
4. according to described method arbitrary in claim 1-3, it is characterised in that: in described chemical vapor deposition step, the time is 2-8 hour;
Pressure is 0-1.01 × 105Pa, but be not 0;
Temperature is 1000-1250 DEG C.
5. according to described method arbitrary in claim 1-4, it is characterised in that: described method also comprises the steps:
Before described chemical vapor deposition step, described substrate is annealed.
6. method according to claim 5, it is characterised in that: in described annealing steps, the atmosphere of annealing is hydrogen and argon gas atmosphere;
The flow of hydrogen is 10-100sccm;
The flow of argon is 10-100sccm;
The time of annealing is 10-60 minute.
7. the three-dimensional grapheme that in claim 1-6, arbitrary described method prepares.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106324291A (en) * | 2016-08-15 | 2017-01-11 | 清华大学 | Graphene film ball probe for atomic force microscopes and method of acquiring friction coefficient |
| CN106323867A (en) * | 2016-08-15 | 2017-01-11 | 清华大学 | Preparation method of graphene membrane spheres |
| CN107452841A (en) * | 2017-09-04 | 2017-12-08 | 湘能华磊光电股份有限公司 | LED epitaxial growth methods based on graphene |
| CN109502575A (en) * | 2018-12-25 | 2019-03-22 | 江苏鲁汶仪器有限公司 | A kind of method of chemical vapor deposition preparation large-area graphene |
| CN109850908A (en) * | 2019-04-12 | 2019-06-07 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and product of silica/graphene complex |
| CN110342502A (en) * | 2019-06-26 | 2019-10-18 | 上海交通大学 | A kind of preparation method of graphite flake growth in situ graphene complex carbon material |
| CN110354700A (en) * | 2018-04-11 | 2019-10-22 | 广州墨羲科技有限公司 | A kind of polymer graphite alkene composite filtering film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106324291A (en) * | 2016-08-15 | 2017-01-11 | 清华大学 | Graphene film ball probe for atomic force microscopes and method of acquiring friction coefficient |
| CN106323867A (en) * | 2016-08-15 | 2017-01-11 | 清华大学 | Preparation method of graphene membrane spheres |
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| CN110354700A (en) * | 2018-04-11 | 2019-10-22 | 广州墨羲科技有限公司 | A kind of polymer graphite alkene composite filtering film |
| CN109502575A (en) * | 2018-12-25 | 2019-03-22 | 江苏鲁汶仪器有限公司 | A kind of method of chemical vapor deposition preparation large-area graphene |
| 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 |
| CN109850908A (en) * | 2019-04-12 | 2019-06-07 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and product of silica/graphene complex |
| 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 |
| CN110342502A (en) * | 2019-06-26 | 2019-10-18 | 上海交通大学 | A kind of preparation method of graphite flake growth in situ graphene complex carbon material |
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