CN107354446A - A kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet - Google Patents

A kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet Download PDF

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Publication number
CN107354446A
CN107354446A CN201710529303.6A CN201710529303A CN107354446A CN 107354446 A CN107354446 A CN 107354446A CN 201710529303 A CN201710529303 A CN 201710529303A CN 107354446 A CN107354446 A CN 107354446A
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passed
tube furnace
ultra
carbon nanosheet
thin carbon
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CN107354446B (en
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阎兴斌
陈江涛
杨兵军
程斌斌
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching

Abstract

The invention discloses a kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet.The present invention uses solid catalyst template, and gas phase carbon source synthesizes ultra-thin carbon nanosheet, and carbon nanosheet size is big, thickness is small.Ultra-thin carbon nanosheet can be used for lithium ion battery and sodium-ion battery equal energy source memory device.

Description

A kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet
Technical field
The present invention relates to a kind of method that ultra-thin carbon nanosheet is prepared using chemical vapor synthesis technology, and in particular to a kind of The method for synthesizing ultra-thin carbon nanosheet using solid catalyst template and gas phase carbon source, belong to carbon material synthesis field.
Background technology
Two-dimentional carbon material has unique structure and excellent physicochemical characteristics, such as larger specific surface area, well Conductive and heat-conductive and mechanical performance, have in fields such as photoelectric device, composite, biology sensor especially energy storage devices huge Big application prospect.At present, Two-dimensional Carbon material preparation method mainly includes mechanical stripping method, chemistry redox technology and change Learn gas phase deposition technology.Although mechanical stripping method can obtain the graphene of high quality and electric property is excellent, yield poorly, no It is adapted to prepare with scale；Although graphite oxidation reduction technique can be prepared with magnanimity, obtained two-dimensional material fault of construction is more, Degree of graphitization is low, mechanical performance and poorly conductive, and during use strong acid, strong oxidizer and reducing agent, process is cumbersome, dirty Contaminate larger；Use, yield need to be shifted as catalysts template chemical vapor deposition preparation process harshness using metal such as copper foil etc. Low, unsuitable magnanimity production；And two-dimentional carbon nanomaterial is prepared as template using metal oxide, need also exist for beforehand through Sequence of chemical reaction prepares nanostructured oxide, then carry out Two-dimensional Carbon materials synthesis [vertical graphene nanometer sheet composition it is more The micro- rod of hole hierarchy carbon and its lithium ion battery applications,《Materials chemistry magazine A》, 2015, volume 3, page 19800]；Adopt By the use of diatomite as template growth two dimension carbon material, during not only need to carry out diatomite the pre-etching of nitric acid and sulfuric acid, Also need to remove template [the bionical template CVD of three-dimensional grapheme powder using hydrofluoric acid or highly basic after 1000 DEG C of growths of high temperature Prepare：Lead to high-efficient solution processing,《Naturally communicate》, 2016, volume 7, page 13440], process is complicated, and pollution is big.Open Hair technique is simple, cost is low and green Two-dimensional Carbon material preparation method is the key for enabling it to be applied in each field.
The content of the invention
It is simple it is an object of the invention to provide a kind of pollution-free, inexpensive, technique and be easy to two-dimensional ultrathin prepared by batch Carbon nanosheet raw powder's production technology.
The present invention use solid catalyst template, and gas phase carbon source synthesizes ultra-thin carbon nanosheet, gained carbon nanosheet size greatly, Thickness is small, being capable of the preparation of scale magnanimity.
A kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet, it is characterised in that this method synthesizes in vacuum tube furnace Ultra-thin carbon nanosheet, vacuum tube furnace are mainly made up of vacuum system, air supply system, heating control system, and detailed process is：
1）Solid catalyst template is placed in vacuum tube furnace；
2）Vacuum tube furnace is evacuated to below 200Pa, inert gas or argon hydrogen gaseous mixture is passed through to atmospheric pressure, is warming up to conjunction Into temperature, and gas phase carbon source is passed through, is cooled to room temperature under atmosphere protection after end of synthesis, obtains solid product；
3）Above-mentioned solid is washed, filtered, is dried to obtain ultra-thin carbon nanosheet powder.
Solid catalyst template of the present invention is lithium carbonate, sodium carbonate, potassium carbonate, potassium chloride, sodium chloride, sodium sulphate Or potassium sulfate.
Gas phase carbon source of the present invention is selected from acetylene, ethene or methane.
Synthesis temperature of the present invention is 600-900 DEG C, generated time 1-150min.
Ultra-thin carbon nanosheet prepared by the present invention is two-dimensional layered structure, and size is in 5-50 μm, thickness 2-30nm.
The invention has the advantages that：
1）Used solid catalyst template is cheap, is not required to pre-process；
2）Synthesis temperature is low, easy to operate controllable, reproducible；
3）Cleaned using deionized water, during without using strong acid/weak base, it is environment-friendly, pollution-free.
The effect benefit of the present invention：Provide a kind of method that simple scale prepares ultra-thin carbon nanosheet, original used in preparation Material is abundant, cheap and easy to get, environment-friendly, reproducible, stable and reliable product quality；Open a kind of new two-dimensional ultrathin carbon Nanometer piece preparation method, prepared ultra-thin carbon nanosheet can be used for lithium ion battery and sodium-ion battery equal energy source memory device.
Brief description of the drawings
Fig. 1 is the TEM photos of the ultra-thin carbon nanosheet of gained in the embodiment of the present invention 4.
Fig. 2 is the Raman collection of illustrative plates of the ultra-thin carbon nanosheet of gained in the embodiment of the present invention 4.
Embodiment
Embodiment 1
Sodium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, argon gas is passed through to atmospheric pressure and is passed through hydrogen Gas（For the 20% of argon gas volume）, tube furnace is warming up to 750 DEG C, is passed through acetylene（For the 20% of hydrogen volume）, 40min is incubated, Stopping is passed through acetylene, after naturally cooling to room temperature, takes out sample, washs above-mentioned solid sample using deionized water, filters simultaneously Ultra-thin carbon nanosheet powder is obtained after 60 DEG C of drying.ESEM（SEM）As a result show that sample has large-size.
Embodiment 2
Sodium chloride powder is placed in vacuum tube furnace, is evacuated to below 200Pa, argon gas is passed through to atmospheric pressure, by tube furnace 700 DEG C are warming up to, is passed through acetylene（For the 5% of argon gas volume）, 40min is incubated, stopping is passed through acetylene, after naturally cooling to room temperature, Take out solid sample.Above-mentioned solid sample is washed using deionized water, filtered and obtains ultra-thin carbon nanometer after 60 DEG C of drying Piece powder.
Embodiment 3
Potassium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through argon gas to atmospheric pressure, be subsequently passed Hydrogen（For the 20% of argon gas volume）, tube furnace is warming up to 850 DEG C, is passed through acetylene（For the 20% of hydrogen volume）, insulation 40min, stopping is passed through acetylene, after naturally cooling to room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water Wash, filter and obtain ultra-thin carbon nanosheet powder after 60 DEG C of drying.
Embodiment 4
Weigh sodium carbonate powder to be placed in vacuum tube furnace, be evacuated to below 200Pa, be passed through argon gas and lead to atmospheric pressure, then Enter hydrogen（For the 20% of argon gas volume）, tube furnace is warming up to 800 DEG C, is passed through acetylene（For the 20% of hydrogen volume）, insulation 40min, stopping is passed through acetylene, after natural cooling is down to room temperature, takes out solid sample.Using deionized water by above-mentioned solid sample Washing, filter and obtain ultra-thin carbon nanosheet powder after 60 DEG C of drying.Fig. 1 is transmission electron microscope（TEM）Figure, as a result shows sample Thickness is smaller, understands that its thickness in 4nm, passes through Raman spectrum by AFM test（Raman, Fig. 2）Test is understood With certain crystallization property.
Embodiment 5
Potassium sulfate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through argon gas to atmospheric pressure, be subsequently passed Hydrogen（For the 20% of argon gas volume）, tube furnace is warming up to 800 DEG C, is passed through acetylene（For the 20% of hydrogen volume）, insulation 40min, stopping is passed through acetylene, after naturally cooling to room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water Wash, filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying, TEM results, which are shown, has obvious two-dimensional slice structure.
Embodiment 6
Sodium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through argon gas to atmospheric pressure, be subsequently passed Hydrogen（For the 10% of argon gas volume）, tube furnace is warming up to 650 DEG C, is passed through acetylene（For the 5% of hydrogen volume）, insulation 150min, stopping is passed through acetylene, after naturally cooling to room temperature, takes out solid sample.Using deionized water by above-mentioned solid sample Washing, filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying.SEM results show that sample has good lamella knot Structure.
Embodiment 7
Carbonic acid powder for lithium is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through nitrogen to atmospheric pressure, be subsequently passed Hydrogen（For the 10% of nitrogen volume）, tube furnace is warming up to 600 DEG C, is passed through acetylene（For the 5% of hydrogen volume）, it is incubated 10min. Then, stop being passed through acetylene, after naturally cooling to room temperature, take out solid sample.Above-mentioned solid sample is washed using deionized water Wash, filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying.ESEM（SEM）As a result show that sample has well Lamellar structure.
Embodiment 8
Potassium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through nitrogen to atmospheric pressure, be subsequently passed Hydrogen（For the 20% of nitrogen volume）, tube furnace is warming up to 900 DEG C, is passed through acetylene（For the 20% of hydrogen volume）, 2min is incubated, Stopping is passed through acetylene, after naturally cooling to room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water, taken out Filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying, TEM results, which are shown, has obvious ultra-thin two-dimension lamellar structure.
Embodiment 9
Potassium chloride powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through nitrogen to atmospheric pressure, be subsequently passed Hydrogen（For the 20% of nitrogen volume）, tube furnace is warming up to 880 DEG C, is passed through methane（For the 50% of hydrogen volume）, insulation 10min, stopping is passed through methane, after naturally cooling to room temperature, takes out solid sample.Above-mentioned solid sample is washed using deionized water Wash, filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying, TEM results, which are shown, has obvious ultra-thin two-dimension lamella knot Structure.
Embodiment 10
Sodium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, be passed through nitrogen to atmospheric pressure, be subsequently passed Hydrogen（For the 30% of nitrogen volume）, tube furnace is warming up to 880 DEG C, is passed through ethene（For the 20% of hydrogen volume）, it is incubated 2min. Then, stop being passed through ethene, after naturally cooling to room temperature, take out solid sample.Above-mentioned solid sample is washed using deionized water Wash, filter and obtain ultra-thin carbon nanosheet powder after 80 DEG C of drying, TEM results, which are shown, has obvious ultra-thin two-dimension lamella knot Structure.
Embodiment 11
Potassium carbonate powder is placed in vacuum tube furnace, is evacuated to below 200Pa, nitrogen is passed through to atmospheric pressure, by tube furnace 880 DEG C are warming up to, is passed through ethene（For the 10% of nitrogen volume）, 60min is incubated, stopping is passed through ethene, naturally cools to room temperature Afterwards, solid sample is taken out.Above-mentioned solid sample is washed using deionized water, filtered and obtains ultra-thin carbon after 80 DEG C of drying and is received Rice piece powder, TEM results, which are shown, has obvious two-dimensional slice structure.

Claims (4)

1. a kind of method that chemical gaseous phase synthesizes ultra-thin carbon nanosheet, it is characterised in that this method synthesizes super in vacuum tube furnace Thin carbon nanosheet, vacuum tube furnace are mainly made up of vacuum system, air supply system, heating control system, and detailed process is：
1）Solid catalyst template is placed in vacuum tube furnace；
2）Vacuum tube furnace is evacuated to below 200Pa, inert gas or argon hydrogen gaseous mixture is passed through to atmospheric pressure, is warming up to conjunction Into temperature, and gas phase carbon source is passed through, is cooled to room temperature under atmosphere protection after end of synthesis, obtains solid product；
3）Above-mentioned solid is washed, filtered, is dried to obtain ultra-thin carbon nanosheet powder.
2. the method as described in claim 1, it is characterised in that solid catalyst template is lithium carbonate, sodium carbonate, potassium carbonate, chlorine Change potassium, sodium chloride, sodium sulphate or potassium sulfate.
3. the method as described in claim 1, it is characterised in that gas phase carbon source is selected from acetylene, ethene or methane.
4. the method as described in claim 1, it is characterised in that synthesis temperature is 600-900 DEG C, generated time 1-150min.
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Cited By (1)

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CN102534544A (en) * 2010-12-14 2012-07-04 财团法人工业技术研究院 Carbon nanotube composite material and its preparation method
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109449440A (en) * 2018-10-31 2019-03-08 武汉理工大学 Ultra-thin soft carbon nanometer sheet of micropore and its preparation method and application
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