CN102212794B - Copper plating substrate-based method for preparing large-area graphene film - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000758 substrate Substances 0.000 title claims abstract description 39
- 239000010949 copper Substances 0.000 title claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000007747 plating Methods 0.000 title abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 22
- 238000009713 electroplating Methods 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 17
- 230000012010 growth Effects 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 229920002120 photoresistant polymer Polymers 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims 2
- 238000004544 sputter deposition Methods 0.000 claims 2
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 238000001465 metallisation Methods 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012159 carrier gas Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000011889 copper foil Substances 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000003292 glue Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000001259 photo etching Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing graphene on a copper plating substrate. The method is characterized by comprising the following steps of: preparing the graphical copper plating substrate on a silicon chip; and growing the graphene on the copper plating substrate for 2 to 5 minutes at the temperature of between 800 and 1,000 DEG C by using a normal pressure chemical vapor deposition method, using methane as a carbon source and using argon and hydrogen as carrier gases. A graphical graphene film can be directly prepared by the method, and the substrate can be compatible with an integrated circuit (IC) process; and the manufacturing method is simple and low in cost, and can be used for large-scale manufacture.
Description
Technical field
The present invention relates to a kind of method that can make graphene film on a large scale, relate to a kind of method or rather, belong to the preparation field of graphene film based on electro-coppering substrate preparation big area graphene film.
Background technology
Graphene is the graphite of individual layer, is that carbon atom in one plane is the material that honey-combed is arranged, and once once is being considered to rationalistic material, because think that it can not stable existence.But after people such as Geim had found self-existent Graphene in 2004, there are some cut-and-try works to verify that the current carrier in the Graphene is the dirac fermion that does not have rest mass in succession, from then on begun the research boom of Graphene.
At present, Graphene be proved to be nano electron device, single-electronic transistor, thermoelectric aspect, there is good prospects for application aspect such as conductive film.But how preparing the large-area graphene film of high quality on a large scale still is a difficult problem, and the method for the Graphene of growing at present mainly contains: the mechanically peel method, and the Graphene quality that obtains is high but area is little, and efficient is also very low; Oxidation reduction process, simple to operate and cost is low, but Graphene can cause the disappearance of some physical and chemical performances in redox processes, and resulting Graphene area is also very little; The silit cracking process can obtain large-area Graphene, but the quality of Graphene receives substrate effects very big, and the growth cost is also higher, needs the high-temperature vacuum environment; Chemical Vapor deposition process is fit to the mass preparation Graphene, but receives the constraint of metal substrate bigger.
Metal substrate commonly used has Cu, Ni, Ru or the like in the chemical Vapor deposition process at present; For the Cu substrate; Be mainly two kinds of sputter copper or Copper Foils on the silicon chip; But these two kinds of Cu substrates all have certain defective in the preparation process: sputter copper at high temperature condenses into the island particle easily, the preparation and the Graphene area too little; The Copper Foil generation gauffer that in operating process, bends easily, thus the planarization of substrate influenced.
The present invention intend propose a kind of based on the electro-coppering substrate, can with the IC process compatible, and the high Graphene growth method of preparation efficiency has solved in the past Graphene and has prepared problems such as graphical difficulty in the process, substrate rapid wear, area are little.
Summary of the invention
The present invention relates to a kind of method based on electro-coppering substrate preparation big area Graphene.The method that is provided comprises that at first a kind of graphical plating of the Graphene that can be used for growing makes.Method based on electro-coppering substrate preparation big area Graphene specifically provided by the invention comprises following two modes:
Method A: step is
1. the preparation of electro-coppering Seed Layer: at SiO
2Substrate or the direct metal seed layer of sputter 50-250nm on silicon base, the material of Seed Layer can be Cu, Ni/Cu, Au, Cr/Au, TiW/Cu etc.;
2. the image conversion of Seed Layer: the thickness according to required electro-coppering is coated with thick glue with Seed Layer, and the thickness of roaring is 4-12 μ m, and then required figure when it is photo-etched into the subsequent growth Graphene;
3. electro-coppering:, select different electroplating currents (0.5-2.5A) and electroplating time (10-100min) according to the thickness (2-10 μ m) of required electro-coppering;
4. remove photoresist, the burn into scribing: with the SiO that has electroplated copper in the step 3
2Substrate or silicon base are removed photoresist material, erode Seed Layer again, just stay the required electro-coppering figure of growth Graphene, again it are divided into suitable size as substrate;
5. the preparation of Graphene: adopt the atmospheric pressure cvd method to use quartz boat to load above-mentioned steps 4 described substrates and put into the silica tube flat-temperature zone of caliber as 60mm; Normal pressure is heated to 800-1000 ℃ under argon gas atmosphere, and argon flow amount is 50-500sccm (mL/min); Feeding carbon-source gas methane and volume ratio are 10 when reaching target temperature in waiting to manage: 1-1: 4 argon gas and hydrogen gas mixture; Behind the growth 3-15min, close heating, methane and argon gas, furnace cooling under argon gas atmosphere, argon flow amount are 50-500sccm.
Method B: it is graphical just to omit step 2 Seed Layer, and all the other are with method A.
Advantage of the present invention is following:
1. the present invention can electroplate out corresponding copper substrate pattern according to the pattern of required Graphene, and the Graphene of directly growing in the above then is with respect to the image conversion method after the film forming, more simple and convenient by method provided by the invention;
2. the present invention is with respect to growth Graphene on Copper Foil, and this method does not receive the influence of extraneous power, and electro-coppering is attached to SiO
2On substrate or the monocrystal silicon substrate, taking of substrate can not have influence on the quality of electro-coppering in the whole process, and Copper Foil just is easy to be damaged;
3. the present invention has avoided the sputter copper film in high-temperature annealing process, can be condensed into the problem of island with respect to growth Graphene on sputter copper, utilizes the Graphene of the inventive method growth, and surface finish height and area are bigger;
4. in technology realizes, electro-coppering cost with respect to the thick copper film of sputter is low, and realization property is high.
5. the present invention can directly prepare patterned graphene film, and substrate can with the IC process compatible, have that method is simple, cost is low, and a characteristic that can mass preparation.
Description of drawings
Fig. 1 (a) is that embodiment 1 electroplates the Cu optical picture behind the Graphene of having grown; (b) be the Raman spectrogram of the Graphene of embodiment 1 growth.
Fig. 2 (a) is that embodiment 2 electroplates the Cu optical picture behind the Graphene of having grown; (b) be the Raman spectrogram of the Graphene of embodiment 2 growths.
Fig. 3 (a) is photoetching section and the striate region of embodiment 3; (b) be the substrate synoptic diagram that image is divided into corresponding size shown in the embodiment 3.
Among the figure:
Embodiment
Embodiment 1: based on electro-coppering substrate preparation big area graphene film
The manufacture craft process is following:
1. with the SiO of silicon single crystal oxidation 200nm
2Zone of oxidation, the Seed Layer of sputter 50nmNi/200nmCu on zone of oxidation again;
2. on above-mentioned silicon chip Seed Layer, electroplate the thick copper of 4 μ m, electroplating current 2A, electroplating time 18min;
3. silicon chip is divided into the size of required substrate, is written into quartz boat, put into the flat-temperature zone of silica tube, under the atmosphere of 300sccm argon gas, be warming up to 1000 ℃;
4. when arriving 1000 ℃ of target temperatures, feed 10sccm methane, 200sccm hydrogen and 800sccm argon gas, behind the growth 3min, under the atmosphere of 200sccm argon gas,, just can make large-area graphene film with furnace annealing.Experimental result is shown in the following figure: wherein Fig. 1 (a) is the optical imagery after growing; Fig. 1 (b) clearlys show that from Raman spectrum Graphene is an individual layer for Raman spectrum.
Embodiment 2: based on electro-coppering substrate preparation multi-layer graphene film
4. when arriving 800 ℃ of target temperatures, feed 15sccm methane, 100sccm hydrogen and 400sccm argon gas, behind the growth 5min, under the atmosphere of 200sccm argon gas,, just can make the multiwalled Graphene with furnace annealing.Experimental result is shown in the following figure: wherein Fig. 2 (a) is the optical imagery after growing; Fig. 2 (b) is a Raman spectrum, and Raman spectrum shows that Graphene is a multilayer.
Embodiment 3: based on the high striated graphene film of electro-coppering substrate preparation
Step 1 is identical with embodiment 1 step 1;
2. Seed Layer is graphical: reticle is illustrated in fig. 1 shown below, and fringe area is the zone (2 μ m * 10 μ m) of electro-coppering, is coated with photoetching behind the thick glue of 5 μ m, develops;
3. electro-coppering: electroplating current 1.8A, electroplating time 15min, electro-coppering thickness 3.5um;
4. remove photoresist material after electroplating, in the mixing solutions of dilute sulphuric acid and ydrogen peroxide 50, soaked tens of seconds again after the cleaning, remove Seed Layer Ni/Cu, clean the back is divided into corresponding size according to image substrate (substrat structure is illustrated in fig. 5 shown below);
Embodiment 3: based on the high striated graphene film of electro-coppering substrate preparation
Step 1 is identical with embodiment 1 step 1;
2. Seed Layer is graphical: shown in following Fig. 3 of reticle (a), fringe area is the zone (2 μ m * 10 μ m) of electro-coppering, is coated with photoetching behind the thick glue of 5 μ m, develops;
3. electro-coppering: electroplating current 1.8A, electroplating time 15min, electro-coppering thickness 3.5um;
4. remove photoresist material after electroplating, in the mixing solutions of dilute sulphuric acid and ydrogen peroxide 50, soaked tens of seconds again after the cleaning, remove Seed Layer Ni/Cu, clean the back is divided into corresponding size according to image substrate (substrat structure is illustrated in fig. 5 shown below);
5. will be written into quartz boat, put into the flat-temperature zone of silica tube, under the atmosphere of 300sccm argon gas; Be warming up to 1000 ℃; When reaching 1000 ℃ of target temperatures, feed 10sccm methane, 200sccm hydrogen and 600sccm argon gas, behind the growth 3min; Under the atmosphere of 200sccm argon gas,, just can make the graphene film of striated with furnace annealing.
Claims (4)
1. method based on electro-coppering substrate preparation big area Graphene is characterized in that adopting in two kinds of methods of A or B any:
Method A:
(a) electro-coppering Seed Layer is at SiO
2Splash-proofing sputtering metal Seed Layer on substrate or the silicon base, seed layer materials are Cu, Ni/Cu, Au, Cr/Au or TiW/Cu;
(b) copper electroplating layer on Seed Layer selects the electroplating current of 0.5-2.5A and the electroplating time of 10-100min to electroplate copper electroplating layer, and the thickness of copper electroplating layer is 2-10 μ m;
(c) substrate that remove photoresist, burn into is diced into suitable size is written into quartz boat; Under nitrogen atmosphere, adopt the atmospheric pressure cvd method; Be heated to 800-1000 ℃; After after reaching target temperature, feeding the mixed gas growth 3-15min of carbon-source gas methane and Ar gas and hydrogen, stop heating and close methane and hydrogen;
(d) furnace cooling under argon atmospher;
Method B:
(a) electro-coppering Seed Layer is at SiO
2Splash-proofing sputtering metal Seed Layer on substrate or the silicon base, seed layer materials are Cu, Ni/Cu, Au, Cr/Au or TiW/Cu;
(b) Seed Layer image conversion: the thickness according to required electro-coppering is coated with one deck photoresist material with Seed Layer, and the thickness of photoresist material is 4-12 μ m, and then it is photo-etched into the required figure of subsequent growth Graphene;
(c) copper electroplating layer on Seed Layer selects the electroplating current of 0.5-2.5A and the electroplating time of 10-100min to electroplate copper electroplating layer, and the thickness of copper electroplating layer is 2-10 μ m;
(d) substrate that remove photoresist, burn into is diced into suitable size is written into quartz boat; Under nitrogen atmosphere, adopt the atmospheric pressure cvd method; Be heated to 800-1000 ℃; After reaching the mixed gas growth 3-15min that feeds carbon-source gas methane and Ar gas and hydrogen under the target temperature, stop heating and close methane and hydrogen;
(e) furnace cooling under argon atmospher;
Wherein, the carbon-source gas that feeds when reaching 800-1000 ℃ of target temperature is a methane, and the flow of methane is 5-20mL/min; The Ar and the H that feed when reaching 800-1000 ℃ of target temperature
2The volume ratio of mixed gas is 10: 1-1: 4.
2. by the described method of claim 1, it is characterized in that:
(1) the seed metallization layer thickness of step (a) sputter is 50-250nm among method A and the B;
(2) among the method A among step (c) and the method B step (d) flow of hydrogen when reaching target temperature be 50-500mL/min;
(3) flow of argon gas is 50-500mL/min during the described furnace cooling of method A step (d) and method B step (e).
3. by claim 1 or 2 described methods, it is characterized in that the graphene film for preparing is a single or multiple lift.
4. by claim 1 or 2 described methods, it is characterized in that the graphene film for preparing is a striated.
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| US9150418B2 (en) * | 2012-02-24 | 2015-10-06 | California Institute Of Technology | Method and system for graphene formation |
| CN102653885A (en) * | 2012-05-22 | 2012-09-05 | 西安电子科技大学 | Method for preparing structured graphene on 3C-SiC substrate |
| CN102718207A (en) * | 2012-05-22 | 2012-10-10 | 西安电子科技大学 | Preparation method of structured grapheme based on Cu membrane annealing and Cl2 reaction |
| CN102674330A (en) * | 2012-05-22 | 2012-09-19 | 西安电子科技大学 | Method for preparing structured graphene on SiC substrate based on Cu film annealing |
| CN103668447B (en) * | 2012-09-01 | 2016-08-31 | 董国材 | A kind of preparation has the identical or preparation facilities of closer crystal lattice orientation Graphene and method |
| CN102881841B (en) * | 2012-10-16 | 2016-01-20 | 北京大学 | With the semiconductor photoelectric device that copper/graphene combination electrode is anode |
| CN103387230B (en) * | 2013-07-23 | 2015-12-23 | 中国科学院微电子研究所 | A kind of preparation method of graphene conductive film |
| CN103529099B (en) * | 2013-09-23 | 2016-06-29 | 西南交通大学 | A kind of growth in situ prepares the method for Graphene chemically modified electrode |
| CN103613094B (en) * | 2013-11-28 | 2016-08-17 | 华中科技大学 | A kind of method simultaneously preparing Graphene and porous amorphous carbon film |
| CN103590099B (en) * | 2013-12-03 | 2016-05-25 | 西安电子科技大学 | The controlled epitaxy method of wafer level Graphene based on MOCVD equipment |
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| US10233566B2 (en) | 2016-12-29 | 2019-03-19 | Ut-Battelle, Llc | Continuous single crystal growth of graphene |
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