CN107215859A - A kind of method of PECVD synthesizing graphite alkene - Google Patents
A kind of method of PECVD synthesizing graphite alkene Download PDFInfo
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- CN107215859A CN107215859A CN201710529296.XA CN201710529296A CN107215859A CN 107215859 A CN107215859 A CN 107215859A CN 201710529296 A CN201710529296 A CN 201710529296A CN 107215859 A CN107215859 A CN 107215859A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of method of PECVD synthesizing graphite alkene.The present invention use solid catalyst template, N doping gas and gaseous carbon sources for raw material, and plasma enhanced chemical low-temperature gaseous phase is synthesized, and scrubbed, suction filtration and is dried to obtain doped or undoped graphene, gained graphene thickness is small, advantages of good crystallization the characteristics of.The present invention has the characteristics of pollution-free, cost is low, process is simple.
Description
Technical field
The present invention relates to the preparation field of graphene, and in particular to a kind of PECVD synthesizing graphite alkene
Method.
Background technology
Graphene was proposed first from seminar of University of Manchester in 2004（Graphene）Concept since, individual layer sp2
The graphene that hydridization carbon is constituted has obtained the height weight of physics, chemistry and material scholar as a bright star of carbon family
Depending on.Similar with single-walled carbon nanotube, graphene has superelevation electrical conductivity, the electric transmission speed that is exceedingly fast, high rigidity, high-ratio surface
Product and room-temperature quantum Hall effect, in the fields such as electron transport device, electrode capacitance device, sensor and composite
There is good application prospect.At present, graphene preparation method mainly include mechanical stripping method, chemistry redox technology and
Chemical vapour deposition technique.Wherein, although mechanical stripping method results in high-quality graphene film and electric property is excellent,
Yield is extremely low, is not suitable for prepare with scale；Graphene is prepared using wet ball grinding technology, although yield is higher, during it is big
Amount uses organic solvent [a kind of method for producing graphene, number of patent application：200910193873.8]；Graphite oxidation reduces skill
Although art can be prepared with magnanimity, obtained graphene-structured defect is more, degree of graphitization is low, mechanical performance and electric conductivity
Difference, and during use strong acid, strong oxidizer and reducing agent, process is cumbersome, pollution is larger；It is used as and is urged using metal such as copper foil etc.
Agent template conventional chemical vapor preparation process harshness is, it is necessary to high temperature（About 1000 DEG C）And used after need to shifting, low yield,
Be not suitable for magnanimity production；And use metal oxide as template and prepare two-dimentional carbon nanomaterial, need also exist in advance by being
Row chemical reaction prepares nano-oxide, then carries out the growth of two-dimensional graphene；Template growth stone is used as using diatomite
The two-dimentional carbon material of black alkene can carry out batch growth, however during not only need to carry out diatomite the pre-embossed of nitric acid and sulfuric acid
Erosion is handled, and also needs to remove template [three-dimensional grapheme powder using hydrofluoric acid or highly basic Strong oxdiative sodium after 1000 DEG C of growths of high temperature
It is prepared by the bionical template CVD of body：Lead to high-efficient solution processing,《Naturally communicate》, 2016, volume 7, page 13440].Cause
This, the graphene preparation method that development technology is simple, low temperature is synthesized, cost is low, pollution is small is to make it apply in each field to be able to
The key promoted development.
Plasma enhanced chemical vapor deposition technology depositing temperature is low, and the structure and impact on physical properties to matrix are small,
Gained thickness of sample and homogeneity of ingredients is good, fine and close, adhesive force strong, can prepare various metals, inorganic and organic film.Using this
Technology, processing machinery and function C film can include diamond-film-like, carbon nano pipe array, amorphous carbon in silicon, metallic substrates
Film etc..Equally, can in different metals, silicon chip and oxidation silicon base using plasma enhanced chemical vapor deposition technology
Graphene wall array film is prepared, [radio frequency plasma strengthens chemical vapour deposition technique system available for field electron transmitting device
Standby carbon nm wall and its field emission characteristic,《Applied surface science》, volume 357, page 1, Appl. Surf. Sci. in 2015
2015, 357, 1 ].However, above-mentioned report does not synthesize lamellar structure graphene.
The content of the invention
It is an object of the invention to provide a kind of low temperature, low cost, it is easy to the method that batch prepares graphene powder.
The present invention uses solid catalyst template, using carbonaceous gas as carbon source, and ammonia is that nitrogen doping source carries out plasma
Body enhancing chemical gaseous phase synthesis, by washing, suction filtration and is dried to obtain graphene powder, gained graphene size is big, thickness is small,
Advantage is protruded in terms of scale magnanimity preparation.
A kind of method of PECVD synthesizing graphite alkene, it is characterised in that this method increases in plasma
Synthesizing graphite alkene in extensive chemical vapor- phase synthesis equipment, equipment mainly by vacuum system, plasma trigger power supply, air supply system,
Heating and pressure control system are constituted, and detailed process is：
1）Solid catalyst template is placed in PECVD synthesis device vacuum system；Described solid is urged
One kind in agent stencil-chosen lithium carbonate, sodium carbonate, potassium carbonate, potassium chloride, sodium chloride, sodium sulphate or potassium sulfate；
2）Vacuum system is evacuated to 10-3Below handkerchief, inert gas or inertia/reproducibility gaseous mixture to 50- are each led into
5000Pa, is warming up to 500-900 DEG C, is passed through gas phase carbon source, or is passed through doped source gas, and doped source gas is ammonia, is passed through
Apply radio frequency or DC source electric discharge build-up of luminance synthesis 0.5-150min, room temperature be cooled under inert gas or reducing gas protection,
Vacuum indoor gas is pumped, atmospheric pressure is inflated to and obtains solid product；
3）By above-mentioned solid washing, suction filtration, it is dried to obtain graphene powder.
Gas phase carbon source of the present invention is selected from acetylene, ethene or methane.
Inert gas of the present invention is nitrogen or argon gas, and reducibility gas is hydrogen.
Plasma of the present invention triggers power supply to be radio frequency or dc source.
Radio-frequency power of the present invention is 50-500W.
DC disruptive voltage of the present invention is 200-800V, and dutycycle is 0.1-0.9.
The graphene that the present invention is synthesized is two-dimensional layered structure, and size is 1-20nm in 1-20 μm, thickness.
The invention has the advantages that：
1）Used solid catalyst template is cheap, is not required to pretreatment；
2）Synthesis temperature is low, advantages of good crystallization, easily doping, reproducible；
3）Cleaning process is washed using distilled water or deionized water, during without using strong acid, highly basic, it is environment-friendly, pollution-free.
The invention provides a kind of simple method for preparing graphene, raw materials are abundant, cheap and easy to get, environment is friendly
Good, reproducible, stable and reliable product quality；Open a kind of method of new low temperature synthesizing graphite alkene.
Brief description of the drawings
Fig. 1 is the TEM photos of gained graphene in the embodiment of the present invention 2.
Fig. 2 is the HR-TEM photos of gained graphene in the embodiment of the present invention 2.
Embodiment
Embodiment 1
Weigh lithium carbonate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 300Pa to be passed through argon gas to pressure in vacuum tank, and lithium carbonate solid is heated into 650 DEG C, hydrogen is passed through（For argon gas volume
120%）And acetylene（For the 20% of hydrogen volume）.Plus radio-frequency power is to 150W, 5min is synthesized, stopping is passed through acetylene, natural cooling
Solid sample is taken out after to room temperature.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after obtain stone
Black alkene powder.Transmission electron microscope（TEM）As a result show that sample has size at 5 μm or so.
Embodiment 2
Weigh sodium carbonate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 300Pa to be passed through argon gas to pressure in vacuum tank, and sodium carbonate solid is heated into 750 DEG C, hydrogen is passed through（For argon gas volume
120%）And acetylene（For the 30% of hydrogen volume）.Plus radio-frequency power is to 150W, 10min is synthesized, stopping is passed through acetylene, natural cooling
Solid sample is taken out after to room temperature.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after obtain stone
Black alkene powder.Fig. 1 and 2 is respectively transmission electron microscope（TEM）And high-resolution-ration transmission electric-lens（HRTEM）Figure, as a result shows that sample has
Large-size, thickness is in 5nm or so.
Embodiment 3
Weigh potash solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 500Pa to be passed through argon gas to pressure in vacuum tank, and potash solid is heated into 850 DEG C, hydrogen is passed through（For argon gas volume
100%）And acetylene（For the 20% of hydrogen volume）.Plus radio-frequency power is to 200W, 100min is synthesized, then stops being passed through acetylene, from
So it is cooled to after room temperature and takes out solid sample.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after
Obtain graphene powder.
Embodiment 4
Weigh sodium carbonate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 300Pa to be passed through argon gas to pressure in vacuum tank, and sodium carbonate solid is heated into 650 DEG C, hydrogen is passed through（For argon gas volume
150%）And acetylene（For the 25% of hydrogen volume）.Plus radio-frequency power is to 150W, 10min is synthesized, then stops being passed through acetylene, from
So it is cooled to after room temperature and takes out solid sample.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after
Obtain graphene powder.TEM results find graphene into big sheet pleated structure.
Embodiment 5
Weigh potassium sulfate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is passed through argon gas and hydrogen（For the 50% of argon gas volume）It is 50Pa to pressure in vacuum tank, potassium sulfate solid is heated to 900 DEG C,
It is passed through ethene（For the 50% of hydrogen volume）.Plus radio-frequency power is to 400W, 3min is synthesized, stopping is passed through ethene, naturally cooled to
After room temperature, solid sample is taken out.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after obtain graphite
Alkene powder.
Embodiment 6
Weigh solid sodium chloride to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is passed through argon gas and hydrogen（For the 100% of argon gas volume）It is 2000Pa to pressure in vacuum tank, solid sodium chloride is heated to 700
DEG C, it is passed through acetylene（For the 25% of hydrogen volume）.Plus radio-frequency power is to 400W, 120min is synthesized, then stops being passed through acetylene, from
So it is cooled to after room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after
Obtain graphene powder.Found by tem observation, graphene thickness is in 10 μm or so, thickness about 10nm or so.
Embodiment 7
Weigh lithium carbonate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 400Pa to be passed through argon gas to pressure in vacuum tank, and lithium carbonate solid is heated into 700 DEG C, hydrogen is passed through（For argon gas volume
100%）And acetylene（For the 25% of hydrogen volume）.Plus DC voltage 500V（Dutycycle 60%）, 20min is synthesized, stopping is passed through second
Alkynes, is naturally cooled to after room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water, suction filtration and at 80 DEG C
Graphene powder is obtained after drying.
Embodiment 8
Weigh sodium sulphate to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Below Pa,
It is 3000Pa to be passed through argon gas to pressure in vacuum tank, and solid sodium sulfate is heated into 900 DEG C, hydrogen is passed through（For argon gas volume
100%）And acetylene（For the 25% of hydrogen volume）.Plus dc power electric discharge synthesis, voltage is 500V（Dutycycle 40%）, synthesis
20min, stopping is passed through acetylene, naturally cools to after room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water
Wash, suction filtration and 80 DEG C dry after obtain graphene powder.
Embodiment 9
Weigh potassium chloride powder to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 800Pa to be passed through nitrogen to pressure in vacuum tank, and solid potassium chloride is heated to rapidly to 600 DEG C, hydrogen is passed through（For nitrogen
The 150% of air volume）And acetylene（For the 20% of hydrogen volume）.Plus DC voltage 800V（Dutycycle 20%）, 10min is synthesized, is stopped
Acetylene is passed through, is naturally cooled to after room temperature, solid sample is taken out.Above-mentioned solid sample is washed using deionized water, suction filtration simultaneously
Graphene powder is obtained after being dried at 80 DEG C.
Embodiment 10
Weigh sodium sulphate powder to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 100Pa to be passed through argon gas to pressure in vacuum tank, and solid sodium sulfate is heated into 600 DEG C, hydrogen is passed through（For argon gas volume
50%）And acetylene（For the 50% of hydrogen volume）.Plus dc power discharge growth, voltage is 400V（Dutycycle 80%）, synthesis
60min, stopping is passed through acetylene, naturally cools to after room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water
Wash, suction filtration and 80 DEG C dry after obtain graphene powder.
Embodiment 11
Weigh sodium carbonate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 300Pa to be passed through argon gas to pressure in vacuum tank, and sodium carbonate solid is heated into 750 DEG C, hydrogen is passed through（For argon gas volume
120%）And acetylene（For the 30% of hydrogen volume）, while being passed through ammonia（For the 50% of hydrogen volume）It is used as doped source.Plus radio frequency work(
Rate synthesizes 5min to 150W, and stopping is passed through acetylene and ammonia, naturally cooled to after room temperature, takes out solid sample.Use deionization
Water washs above-mentioned solid sample, suction filtration and 60 DEG C dry after obtain nitrogen-doped graphene powder, wherein passing through x-ray photoelectricity
Sub- energy spectrum analysis show that nitrogen element content is about 2.5%.
Embodiment 12
Weigh solid sodium chloride to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 300Pa to be passed through argon gas to pressure in vacuum tank, and solid sodium chloride is heated into 650 DEG C, hydrogen is passed through（For argon gas volume
120%）And methane（For the 40% of hydrogen volume）, while being passed through ammonia（For the 20% of hydrogen volume）It is used as doped source.Plus radio frequency work(
Rate synthesizes 20min to 300W, and stopping is passed through methane and ammonia, naturally cooled to after room temperature, takes out solid sample.Using go from
Sub- water washs above-mentioned solid sample, suction filtration and 60 DEG C dry after obtain nitrogen-doped graphene powder, wherein passing through x-ray light
Electron spectroscopy analysis show that nitrogen element content is about 3.0%.
Embodiment 13
Weigh potassium sulfate solid to be placed in PECVD synthesis device vacuum system, be evacuated to 10-3Pa with
Under, it is 1500Pa to be passed through argon gas to pressure in vacuum tank, and potassium sulfate solid is heated into 680 DEG C, hydrogen is passed through（For argon gas volume
50%）And ethene（For the 100% of hydrogen volume）, while being passed through ammonia（For the 40% of hydrogen volume）It is used as doped source.Plus direct current
Press 500V（Dutycycle 60%）, 120min is synthesized, stopping is passed through ethene and ammonia, naturally cooled to after room temperature, takes out solid-like
Product.Above-mentioned solid sample is washed using deionized water, suction filtration and 60 DEG C dry after obtain nitrogen-doped graphene powder.
Claims (6)
1. a kind of method of PECVD synthesizing graphite alkene, it is characterised in that this method is in plasma enhancing
Synthesizing graphite alkene in chemical gaseous phase synthesis device, equipment mainly triggers power supply, air supply system, liter by vacuum system, plasma
Temperature and pressure control system are constituted, and detailed process is：
1）Solid catalyst template is placed in PECVD synthesis device vacuum system；Described solid is urged
One kind in agent stencil-chosen lithium carbonate, sodium carbonate, potassium carbonate, potassium chloride, sodium chloride, sodium sulphate or potassium sulfate；
2）Vacuum system is evacuated to 10-3Below handkerchief, inert gas or inertia/reproducibility gaseous mixture to 50- are each led into
5000Pa, is warming up to 500-900 DEG C, is passed through gas phase carbon source, or is passed through doped source gas, and doped source gas is ammonia, is passed through
Apply radio frequency or DC source electric discharge build-up of luminance synthesis 0.5-150min, room temperature be cooled under inert gas or reducing gas protection,
Vacuum indoor gas is pumped, atmospheric pressure is inflated to and obtains solid product；
3）By above-mentioned solid washing, suction filtration, it is dried to obtain graphene powder.
2. the method as described in claim 1, it is characterised in that gas phase carbon source is selected from acetylene, ethene or methane.
3. the method as described in claim 1, it is characterised in that inert gas is nitrogen or argon gas, and reducibility gas is hydrogen.
4. the method as described in claim 1, it is characterised in that plasma triggers power supply to be radio frequency or dc source.
5. method as claimed in claim 4, it is characterised in that radio-frequency power is 50-500W.
6. method as claimed in claim 4, it is characterised in that DC disruptive voltage is 200-800V, dutycycle is 0.1-0.9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109956462A (en) * | 2019-03-14 | 2019-07-02 | 北京航空航天大学 | Carbon nano-particle preparation system, carbon nano-particle aerosol generate system and method |
| CN110171814A (en) * | 2019-05-13 | 2019-08-27 | 电子科技大学 | Water-soluble KCl catalyzes and synthesizes the method and energy storage, sustained release application of carbon nanosheet |
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Application publication date: 20170929 |