CN105948032A - Method for etching multilayer graphene - Google Patents
Method for etching multilayer graphene Download PDFInfo
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- CN105948032A CN105948032A CN201610520022.XA CN201610520022A CN105948032A CN 105948032 A CN105948032 A CN 105948032A CN 201610520022 A CN201610520022 A CN 201610520022A CN 105948032 A CN105948032 A CN 105948032A
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- layer graphene
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Abstract
The invention relates to a method for etching multilayer graphene. The method comprises the following steps that (1) a cerate water solution is prepared, and the concentration is 0.1 to 0.3mol/L; (2) under the continuous stirring condition, an inorganic base solution, the multilayer graphene and a dispersing agent are added into the solution, and meanwhile, the pH is controlled to be 9 to 10, so that cerium nanoparticles are deposited on the multilayer graphene surface, the continuous stirring is performed for 1 to 2 hours after the reaction completion; (3) the obtained product is filtered, cleaned and dried; (4) the obtained product is annealed at Ar/H2 atmosphere, and the annealing concretely comprises the steps that the temperature rises at a constant speed; the heat insulation temperature is in a range being 800 to 1100 DEG C, and the heat insulation time is 1 to 3 hours; the product is naturally cooled to the room temperature; the Ar/H2 atmosphere is kept unchanged in the processes of temperature rise, heat insulation and temperature reduction; the Ar/H2 flow rate is respectively 100 to 500sccm and 10 to 50sccm.
Description
Technical field
The present invention relates to a kind of method etching Graphene, belong to the lithographic technique field of Graphene.
Background technology
Graphene is one of the primary study object in physics and materialogy field in recent years, and it is strict
Two dimensional crystal, sp2 hydbridized carbon atoms that be bonded and there is the cellular two-dimensional structure of hexagonal lattice.To the greatest extent
The developing history of pipe Graphene is shorter, but the physical property of its excellence and potential application prospect have been drawn
Play the extensive concern of physics circle and region of chemistry, become Condensed Matter Physics and material supply section after CNT
Another study hotspot in field.
Graphene as a kind of be made up of regular hexagon carbocyclic ring infinitely extend crystal, be graphically to be transported
For micro-nano electronic device and the key technology of integrated circuit, Graphene is the semimetal of a kind of zero band gap,
Utilize pattern technology that the graphene nanobelt that Graphene etching becomes nano-width can be opened graphite
Alkene band gap, by pattern technology, also Graphene can be processed into various active, passive device and some
There is the micro structure of specific function.At present, the pattern technology of Graphene has multiple, such as oxygen plasma
Body etching, conduction AFM etching etc., but, the graphene edge that existing lithographic technique etches is not
Smooth, edge defect is very big on material property impact, for the etching of multi-layer graphene, utilizes existing skill
Only all multi-layer graphene crystal is carried out plane machining during art, it is impossible to multi-layer graphene is synchronized, solely
On the spot etch, and the etching in different layers be independent of each other, it is impossible in the case of not destroying other layers,
If optionally a certain layer in multi-layer graphene or dried layer being performed etching.
Summary of the invention
The present invention is directed to the deficiency that existing Graphene lithographic technique exists, it is provided that a kind of etching multi-layer graphene
Method.
The technical scheme is that
A kind of method etching multi-layer graphene, it is characterised in that comprise the steps:
1) preparing the aqueous solution of cerium salt, concentration is 0.1～0.3mol/L；
2) under the conditions of being stirred continuously, to step 1) solution in add inorganic alkali solution, multi-layer graphene and
Dispersant, control pH is 9～10 simultaneously, thus at the nano-particle of the surface of multi-layer graphene deposition cerium,
After reaction terminates, continue stirring 1～2 hour；
3) by step 2) products obtained therefrom filtration, clean, be dried；
4) by step 3) products obtained therefrom is in Ar/H2Anneal under atmosphere, specifically include: at the uniform velocity heat up, insulation temperature
Degree is in the range of 800～1100 DEG C, and temperature retention time is 1～3 hour, naturally cools to room temperature, heat up,
Insulation, temperature-fall period keep Ar/H2Atmosphere is constant, Ar/H2Flow be respectively 100～500sccm
With 10～50sccm.
Further, step 1) described in cerium salt be the one in Cericammoniumsulfate, cerous nitrate, cerous sulfate.
Further, the cerium in described cerium salt is 1:3～1:5 with the weight ratio of multi-layer graphene.
Further, step 2) described in inorganic base be in sodium hydroxide, potassium hydroxide, ammonia
Kind.
Further, step 2) described in dispersant be oligomer of phenylamine.
Further, described dispersant is 1:3～3:1 with the mol ratio of multi-layer graphene.
Further, during described oligomer of phenylamine is aniline trimer, Tetraaniline, aniline pentamer
A kind of.
The invention has the beneficial effects as follows:
1) during cerium oxide nanoparticles is formed, multi-layer graphene is added so that cerium oxide nano
Granule in each position of multi-layer graphene formed, be evenly distributed, thus finally give etched after
Multi-layer graphene flush edge, zero defect, and each layer have carried out synchronization, independent etching, through this method
The multi-layer graphene that process obtains can be used for being processed into various active, passive device and some have specific merit
The micro structure of energy.
2) operating procedure is simple, it is easy to accomplish, low cost, effective, it is suitable for heavy industrialization
Application.
Detailed description of the invention
Being described principle and the feature of the present invention below in conjunction with example, example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.
Embodiment 1:
A kind of method etching multi-layer graphene, comprises the steps:
1) weigh Cericammoniumsulfate 60g to be dissolved in the distilled water of 1000ml, be configured to solution；
2) under the conditions of being stirred continuously, in Cericammoniumsulfate solution, the sodium hydroxide solution of 0.5mol/L is dripped
20ml, adds the multi-layer graphene of 42g and the aniline trimer of 5g while dropping in mixture,
Keeping pH value is 9～10, continues stirring 1 hour after completion of the reaction, makes Graphene and cerium oxide nano
Grain is fully contacted；
3) by step 2) mixture after completion of the reaction filters, cleans with water and acetone respectively, be placed on baking oven
In be dried；
4) dried products obtained therefrom is placed in Ar/H2Anneal under atmosphere, specifically include: with the speed of 5 DEG C/min
At the uniform velocity heating up, holding temperature is at 800 DEG C, and temperature retention time is 2 hours, naturally cools to room temperature, heat up,
Insulation, temperature-fall period keep Ar/H2Atmosphere is constant, Ar/H2Flow be respectively 300sccm and
30sccm。
Embodiment 2:
A kind of method etching multi-layer graphene, comprises the steps:
1) weigh cerous nitrate 43g to be dissolved in the distilled water of 1000ml, be configured to solution；
2) under the conditions of being stirred continuously, in cerous nitrate solution, the potassium hydroxide solution 20ml of 0.5mol/L is dripped,
While dropping, in mixture, add the multi-layer graphene of 60g and the aniline trimer of 10g, keep
PH value is 9～10, continues stirring 2 hours after completion of the reaction, makes Graphene fill with cerium oxide nanoparticles
Tap is touched；
3) by step 2) mixture after completion of the reaction filters, cleans with water and acetone respectively, be placed on baking oven
In be dried；
4) dried products obtained therefrom is placed in Ar/H2Anneal under atmosphere, specifically include: with the speed of 10 DEG C/min
Degree at the uniform velocity heats up, and holding temperature is at 1100 DEG C, and temperature retention time is 2 hours, naturally cools to room temperature, rises
Temperature, insulation, temperature-fall period keep Ar/H2Atmosphere is constant, Ar/H2Flow be respectively 100sccm and
10sccm。
Embodiment 3:
A kind of method etching multi-layer graphene, comprises the steps:
1) weigh cerous sulfate 40g to be dissolved in the distilled water of 1000ml, be configured to solution；
2) under the conditions of being stirred continuously, in cerous nitrate solution, drip the ammonia spirit 20ml of 1mol/L, dripping
In mixture, add the multi-layer graphene of 70g and the aniline trimer of 20g while adding, keep pH
Value is 9～10, continues stirring 2 hours after completion of the reaction, makes Graphene abundant with cerium oxide nanoparticles
Contact；
3) by step 2) mixture after completion of the reaction filters, cleans with water and acetone respectively, be placed on baking oven
In be dried；
4) dried products obtained therefrom is placed in Ar/H2Anneal under atmosphere, specifically include: with the speed of 5 DEG C/min
At the uniform velocity heating up, holding temperature is at 1000 DEG C, and temperature retention time is 3 hours, naturally cools to room temperature, heat up,
Insulation, temperature-fall period keep Ar/H2Atmosphere is constant, Ar/H2Flow be respectively 500sccm and
50sccm。
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (7)
1. the method etching multi-layer graphene, it is characterised in that comprise the steps:
1) preparing the aqueous solution of cerium salt, concentration is 0.1～0.3mol/L；
2) under the conditions of being stirred continuously, to step 1) solution in add inorganic alkali solution, multi-layer graphene and
Dispersant, control pH is 9～10 simultaneously, thus at the nano-particle of the surface of multi-layer graphene deposition cerium,
Reaction continues stirring 1～2 hour after terminating；
3) by step 2) products obtained therefrom filtration, clean, be dried；
4) by step 3) products obtained therefrom is in Ar/H2Anneal under atmosphere, specifically include: at the uniform velocity heat up, insulation temperature
Degree is in the range of 800～1100 DEG C, and temperature retention time is 1～3 hour, naturally cools to room temperature, heat up,
Insulation, temperature-fall period keep Ar/H2Atmosphere is constant, Ar/H2Flow be respectively 100～500sccm
With 10～50sccm.
The method of etching multi-layer graphene the most according to claim 1, it is characterised in that step 1)
Described in cerium salt be the one in Cericammoniumsulfate, cerous nitrate, cerous sulfate.
The method of etching multi-layer graphene the most according to claim 1, it is characterised in that described
Cerium in cerium salt is 1:3～1:5 with the weight ratio of multi-layer graphene.
The method of etching multi-layer graphene the most according to claim 1, it is characterised in that step 2)
Described in inorganic base be the one in sodium hydroxide, potassium hydroxide, ammonia.
The method of etching multi-layer graphene the most according to claim 1, it is characterised in that step 2)
Described in dispersant be oligomer of phenylamine.
The method of etching multi-layer graphene the most according to claim 5, it is characterised in that described
Dispersant is 1:3～3:1 with the mol ratio of multi-layer graphene.
The method of etching multi-layer graphene the most according to claim 6, it is characterised in that described
Oligomer of phenylamine is the one in aniline trimer, Tetraaniline, aniline pentamer.
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| CN201610520022.XA CN105948032A (en) | 2016-07-04 | 2016-07-04 | Method for etching multilayer graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI668188B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device and method for rapidly producing graphene/nano metal oxide composite material |
| CN110698887A (en) * | 2019-08-14 | 2020-01-17 | 哈尔滨工业大学（威海） | CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder |
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|---|---|---|---|---|
| CN102701144A (en) * | 2012-06-25 | 2012-10-03 | 北京大学 | Method for etching multilayer graphene |
| CN103078123A (en) * | 2013-01-08 | 2013-05-01 | 北京化工大学 | Fuel cell catalyst and preparation method thereof |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
| CN105255446A (en) * | 2015-11-06 | 2016-01-20 | 安徽理工大学 | Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof |
| CN105645388A (en) * | 2014-12-02 | 2016-06-08 | 中国科学院宁波材料技术与工程研究所 | Graphene dispersant and applications thereof |
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2016
- 2016-07-04 CN CN201610520022.XA patent/CN105948032A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701144A (en) * | 2012-06-25 | 2012-10-03 | 北京大学 | Method for etching multilayer graphene |
| CN103078123A (en) * | 2013-01-08 | 2013-05-01 | 北京化工大学 | Fuel cell catalyst and preparation method thereof |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
| CN105645388A (en) * | 2014-12-02 | 2016-06-08 | 中国科学院宁波材料技术与工程研究所 | Graphene dispersant and applications thereof |
| CN105255446A (en) * | 2015-11-06 | 2016-01-20 | 安徽理工大学 | Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《ACS NANO》 * |
| 《DALTON TRANS》 * |
| ZBYNEK NOVOTNY ETAL: "Cerium Oxide Nanoclusters on Graphene/Ru(0001): Intercalation of Oxygen via Spillover", 《ACS NANO》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI668188B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device and method for rapidly producing graphene/nano metal oxide composite material |
| CN110698887A (en) * | 2019-08-14 | 2020-01-17 | 哈尔滨工业大学（威海） | CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder |
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Application publication date: 20160921 |