CN103224231A - Transfer method of graphite film - Google Patents
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- CN103224231A CN103224231A CN2013101431819A CN201310143181A CN103224231A CN 103224231 A CN103224231 A CN 103224231A CN 2013101431819 A CN2013101431819 A CN 2013101431819A CN 201310143181 A CN201310143181 A CN 201310143181A CN 103224231 A CN103224231 A CN 103224231A
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Abstract
The invention discloses a transfer method of graphite film, which belongs to the field of material processing. The method aims at graphite prepared on nickel and other metal films by chemical vapor deposition method (CVD), and employs hydrogen bubble generated by reaction of a dilute acid solution and a metal substrate to separate the graphite layer and the metal substrate. PMMA and other polymers are not needed to cover the upper layer of the graphite for transferring carrier according to the invention, so no pollutants are introduced, and damage of graphite surface is greatly reduced; the peeling process is carried out by a direct chemical reaction between the acidic solution and the metal, thereby realizing separation of graphite on the upper and lower surface of the metal film and the metal film simultaneously with high efficiency and without external power source and electrochemical reaction. The invention has a simple operation technology and does not relate to harmful chemical substances. The metal substrate can be used for multitime with repetition, and the cost is greatly reduced. The invention has a large application value in the industrial field for large scale preparation of graphite.
Description
Technical field
The invention belongs to material processing field, be specifically related to a kind of transfer method of multi-layer graphene film.
Background technology
In recent years, Graphene has obtained the extensive concern in scientific research and engineering field as a kind of brand-new material.Graphene (Graphene) is a kind of individual layer sheet nano material that is made of carbon atom, and theoretic throat only is 0.34nm.Its sp
2The C atom of hydridization all forms saturated bond, so Graphene has very high chemical stability and physical strength, and its young's modulus can reach 1.0Tpa, and breaking strength can reach 40N/m.In addition, Graphene has good heat conduction and conductive capability, under the room temperature its resistivity be about～10
-8Ω m, the current density that can carry can reach 10
8A/cm
2Therefore, this material has big application prospect at microelectronic.Graphene can use carbon sources such as methane, ethene usually as a kind of allotropic substance of C element, be that catalyzer synthesizes with copper, nickel, so the cost of mass preparation Graphene is very low, is convenient to suitability for industrialized production.
Graphene has more application in fields such as microelectronic device, nanometer electronic device, molecule sensor, solar cells because of its electroconductibility, visible light transmission, snappiness and physical strength preferably.Because the Graphene of CVD method preparation normally grows on the metal substrate such as copper, nickel, when preparation micro-nano electron device and transmitter, individual layer or multiwalled Graphene need be transferred on the substrates such as silicon, silicon-dioxide, gan.Transfer method commonly used at present is to be the wet method transfer techniques of carrier with PMMA glue or other high molecular polymers.This transfer techniques need cover protective layer and the transfer vector of PMMA glue as graphene film on the good graphene layer of growth.Utilize iron(ic) chloride or ammonium persulfate solution to erode the metal substrate of Graphene bottom then, the graphene layer that will cover PMMA glue is again transferred on the substrates such as silicon-dioxide, gan, utilizes the PMMA layer on the organic solutions removal Graphenes such as acetone, Virahol then.Shift Graphene to different substrates though this method is convenient to big area, bring multiple pollutent and breakage to graphene layer easily.In addition, substrate material also cannot be reused.The cost height is not easy to scale operation.Other reports, the Korea S scientist can utilize a kind of special solid-state adhesive tape as carrier Graphene to be transferred on the soft substrate such as plastics, but this technology still fails to solve the problem of transfer vector pollutent and metal substrate recycling.
Summary of the invention
The objective of the invention is to propose a kind of transfer method of graphene film, can significantly reduce pollution and the destruction of transfer process, and metal substrate can repeatedly be utilized, reduce production costs Graphene.
The transfer method of a kind of graphene film provided by the invention, shifting process is as follows:
1, the pre-treatment of metal substrate:
With the catalyzer of metals such as Ni film, utilize acetone, ethanol and dilute hydrochloric acid process metal surfaces to remove impurity such as metal oxide, greasy dirt as CVD method growth Graphene.
2, utilize the CVD method on above-mentioned metallic film, to prepare Graphene:
Utilize chemical Vapor deposition process, on above-mentioned metallic film, prepare graphene layer.Normally used carbon source is gases such as methane, ethene, acetylene, and other assist gass in the reaction are hydrogen and argon gas, and wherein hydrogen plays reductive action, and argon gas shields.The primitive reaction principle is as shown below, feeds hydrogen and argon gas in the reaction all the time, and hydrogen is used to reduce the oxide compound of metallic surface, and argon gas plays a protective role.After treating that temperature rises a suitable temperature (in 600-1100 ° of C scope), metal heat preservation annealing for some time, feed carbon sources such as methane, ethene or acetylene then.Cracking can take place in carbon-source gas under high temperature action, carbon atom wherein can be grown to Graphene in the metallic surface under the katalysis of metallic copper or nickel.So just, can prepare Graphene on the top layer of metallic film, after equitemperature drops to room temperature then, sample be taken out from Reaktionsofen.
3, remove the lateral graphene layer of metallic film:
The side all can grow Graphene around the upper and lower surface of metallic film reached, and for ease of the reaction of metal substrate and acidic solution in the subsequent transfer process, needed earlier the lateral Graphene of metallic film is removed, and exposed exposed metal.
4, utilize between acidic solution and the metal substrate directly chemical reaction, upper and lower two the lip-deep Graphenes of stripping metal substrate, need not to utilize electrochemical reaction at this process dispense with outer connecting power:
Above-mentioned Graphene-metallic film structure is placed acid solution, and acid solution can slowly generate hydrogen from the fault location of Graphene and taking place with metal of substrate all around.The reactive force of hydrogen can promote metal substrate upper and lower two lip-deep Graphenes slowly to be separated with metal substrate, as shown in Figure 1.
5, shift Graphene to substrate
Graphene after being stripped from can float on solution surface, Graphene is picked up can directly dry and be transferred on the various substrates after placing deionized water to clean.
Ultimate principle of the present invention:
The present invention utilizes the graphene layer of the hydrogen stripping metal substrate upper and lower surface of acidic solution and the generation of metal substrate direct reaction, need not the Graphene transfer method of polymkeric substance (PMMA etc.) as transfer vector.This method can significantly reduce the pollution that carrier such as polymkeric substance brings to Graphene in the transfer process, and substrate can repeatedly be used.And can significantly improve the quality of transferring to the Graphene on the substrate, and can reduce production costs.Therefore, this technology will have big using value in Graphene preparation and transfer party mask.
Advantage of the present invention:
1, Graphene surface no-pollution, the Graphene transfer method of this method design need not transfer vector such as PMMA and are covered in the Graphene upper strata, therefore can not introduce impurity such as polymkeric substance.
2, graphene-structured is complete, because chemical reaction slowly can take place with metal Ni in diluted acid, and the production small quantity of hydrogen, the reactive force of hydrogen gas bubbles slowly promotes Graphene and substrate separation, can not tear Graphene.
3, the present invention is not by means of electrochemical principle, is to utilize chemical reaction, and the Graphene of metal catalyst upper and lower surface can both be stripped down from metal substrate, and can only single face glass by means of the method for electrochemical principle;
4, be convenient to be transferred to multiple substrate, because multi-layer graphene density is less than water, the Graphene after the separation can float on solution surface, just is transferred to different substrates after picking up.
5, substrate can use repeatedly, and the Ni metallic film after peeling off can repeatedly utilize after cleaning, and the growth Graphene reduces production costs.
6, nontoxic, can not relate to poisonous high molecular polymers such as PMMA in the technological process, therefore can not influence operator's health.
Description of drawings
Fig. 1 promotes Graphene and the isolating synoptic diagram of metallic film for the present invention utilizes the reactive force of hydrogen;
Fig. 2 is the synoptic diagram of Graphene and nickel substrate separation in the embodiment of the invention.
Wherein: 1-metallic film; 2-Graphene; 3-oxygen
Embodiment
Illustrate the present invention with embodiment below, but these embodiment should not be interpreted as limitation of the present invention.
With the Graphene that utilizes hydrochloric acid soln to shift the nickel film preparation is example:
1, the pre-treatment of nickel film
With the catalyzer of metal nickel film (50 nanometers-1 millimeter), utilize acetone, ethanol and dilute hydrochloric acid to handle the nickel film surface to remove impurity such as metal oxide, greasy dirt as CVD method growth Graphene.
2, preparing individual layer, bilayer or graphene layer (thickness can reach below the micron) more than three layers on the nickel film.
Utilize chemical Vapor deposition process, on the nickel film, prepare graphene layer.The carbon source of using is methane (CH
4), other assist gass in the reaction are hydrogen H
2And argon Ar, wherein hydrogen plays reductive action, and argon gas shields.
(1) the nickel film after will handling is put into CVD technology tube furnace.
(2) feed hydrogen and argon gas (H
2Flow 25sccm, Ar flow 500sccm), make boiler tube heat up gradually, make boiler tube rise to 1000 ° of C after 40 minutes by room temperature.
(3) when 1000 ° of C, make boiler tube keep constant temperature ten minutes, nickel is carried out anneal.
(4) feed methane (CH
4Flow 15sccm) 5 minutes, makes the boiler tube cooling then.
(5) treat that boiler tube is cooled to room temperature after, take out sample.
3, remove the graphene layer of nickel side surface of thin film
Utilize scissors will wrap up graphite the nickel film around cut, make it expose exposed metal.
4, peel off Graphene and metallic nickel substrate
(1) above-mentioned Graphene-nickel membrane structure is placed the hydrochloric acid 96 hours of 1:1.
(2) Graphene 1 for the treatment of upper and lower surface is with after nickel substrate 2 separates, as shown in Figure 2;
(3) Graphene and metal substrate are picked up respectively.
(4) place deionized water to clean Graphene and metal substrate.
5, shift Graphene to SiO
2Substrate
(1) utilizes SiO
2Substrate picks up Graphene from deionized water.
(2) sample is placed 150 ° of C baking oven oven dry take out after 10 minutes.
Above-described embodiment is used to limit the present invention, and any those skilled in the art without departing from the spirit and scope of the present invention, can do various changes and retouching, except that nickel, can also be iron as metallic film.Therefore protection scope of the present invention is looked the claim scope and is defined.
Claims (4)
1. the transfer method of a Graphene specifically comprises the steps:
1) with the catalyzer of metallic film as the growth Graphene, utilize chemical Vapor deposition process, on metallic film, prepare Graphene, specifically comprise: feed hydrogen and argon gas, after treating that temperature is raised to 600-1100 ° of C, Schilling metal annealing for some time, feed methane, ethene or acetylene carbon source then, cracking can take place in carbon source under high temperature action, the Graphene that under the katalysis of metallic film, has defective then in the metallic film surface growth, after equitemperature drops to room temperature, the metallic film that wraps up Graphene is taken out from Reaktionsofen;
2) remove the lateral Graphene of metallic film;
3) the above-mentioned metallic film structure that has Graphene is put in the acidic solution, realizes that the Graphene on the upper and lower surface of metallic film separates with metallic film simultaneously;
4) Graphene is picked up from solution place deionized water, directly dry after the cleaning and be transferred on the various substrates.
2. the method for claim 1 is characterized in that, the metallic film as catalyzer in the step 1) carries out pre-treatment, promptly utilizes acetone, ethanol and dilute hydrochloric acid to handle the metallic film surface.
3. the method for claim 1 is characterized in that, acidic solution described in the step 3) is a hydrochloric acid, the concentration range 1%-37.5% of hydrochloric acid, 1-200 hour storage period.
4. the method for claim 1 is characterized in that, described metallic film is nickel or iron.
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| CN104016335A (en) * | 2014-05-30 | 2014-09-03 | 无锡格菲电子薄膜科技有限公司 | Graphene transfer method |
| CN104016340A (en) * | 2014-06-30 | 2014-09-03 | 上海集成电路研发中心有限公司 | Method for transferring graphene film |
| CN104030274A (en) * | 2014-05-28 | 2014-09-10 | 中国科学院上海微***与信息技术研究所 | Wet etching chemical transfer method for enhancing surface cleanliness of graphene |
| CN104261389A (en) * | 2014-09-18 | 2015-01-07 | 苏州经贸职业技术学院 | Graphene, and preparation method and application thereof |
| CN104374486A (en) * | 2014-11-13 | 2015-02-25 | 中国科学院重庆绿色智能技术研究院 | Flexible temperature sensor based on graphene nanometer wall and preparing method thereof |
| CN105129785A (en) * | 2015-08-26 | 2015-12-09 | 中国科学院上海微***与信息技术研究所 | Preparation method of graphene on insulator |
| CN106158145A (en) * | 2016-06-24 | 2016-11-23 | 成都天航智虹企业管理咨询有限公司 | A kind of preparation method of graphene conductive film |
| CN106629692A (en) * | 2016-10-18 | 2017-05-10 | 东南大学 | Synchronous transfer method for upper and lower graphene films growing on copper foil surfaces in coated manner |
| CN107915220A (en) * | 2017-11-17 | 2018-04-17 | 合肥国轩高科动力能源有限公司 | A kind of method of gas-liquid interface partition method transfer graphene pattern film |
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