KR101346322B1 - Graphene nanoribbons and method of manufacturing the same and transparent conductive film and electronic device including the graphene nanoribbons - Google Patents
Graphene nanoribbons and method of manufacturing the same and transparent conductive film and electronic device including the graphene nanoribbons Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 239000002074 nanoribbon Substances 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 239000002608 ionic liquid Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000001678 irradiating effect Effects 0.000 claims abstract description 19
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 claims abstract description 11
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 16
- -1 1-ethyl-3-methylimidazolium tetrafluoroborate Chemical compound 0.000 claims description 13
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 claims description 12
- INDFXCHYORWHLQ-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;1-butyl-3-methylimidazol-3-ium Chemical compound CCCCN1C=C[N+](C)=C1.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F INDFXCHYORWHLQ-UHFFFAOYSA-N 0.000 claims description 6
- LRESCJAINPKJTO-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;1-ethyl-3-methylimidazol-3-ium Chemical compound CCN1C=C[N+](C)=C1.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F LRESCJAINPKJTO-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- WGCOTPLCCFYGKV-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium 2,2,2-trifluoroethanesulfonate Chemical compound FC(CS(=O)(=O)[O-])(F)F.C(CCC)[N+]1=CN(C=C1)C WGCOTPLCCFYGKV-UHFFFAOYSA-M 0.000 claims description 3
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims description 3
- BMQZYMYBQZGEEY-UHFFFAOYSA-M 1-ethyl-3-methylimidazolium chloride Chemical compound [Cl-].CCN1C=C[N+](C)=C1 BMQZYMYBQZGEEY-UHFFFAOYSA-M 0.000 claims description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 3
- RHPFAQZSMZNLFV-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium 2,2,2-trifluoroethanesulfonate Chemical compound FC(CS(=O)(=O)[O-])(F)F.C(C)[N+]1=CN(C=C1)C RHPFAQZSMZNLFV-UHFFFAOYSA-M 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000006479 redox reaction Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- XGMDYIYCKWMWLY-UHFFFAOYSA-N 2,2,2-trifluoroethanesulfonic acid Chemical compound OS(=O)(=O)CC(F)(F)F XGMDYIYCKWMWLY-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- C01B32/182—Graphene
- C01B32/184—Preparation
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- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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Abstract
구리 프탈로시아닌 및 이온성 액체를 포함하는 혼합물을 준비하는 단계, 그리고 상기 혼합물에 마이크로웨이브를 조사하는 단계를 포함하는 그래핀 나노 리본의 제조 방법, 상기 방법으로 제조된 그래핀 나노 리본, 상기 그래핀 나노 리본을 포함하는 투명 도전막 및 전자 소자에 관한 것이다.A method of preparing a graphene nano ribbon comprising preparing a mixture comprising copper phthalocyanine and an ionic liquid, and irradiating microwaves to the mixture, a graphene nano ribbon prepared by the method, the graphene nano The present invention relates to a transparent conductive film and an electronic device comprising a ribbon.
Description
그래핀 나노 리본 및 그 제조 방법과 상기 그래핀 나노 리본을 포함하는 투명 도전막 및 전자 소자에 관한 것이다.
The present invention relates to a graphene nano ribbon, a method of manufacturing the same, and a transparent conductive film and an electronic device including the graphene nano ribbon.
일반적으로 표시소자, 발광다이오드, 태양 전지 등과 같은 다양한 전자 소자는 광을 투과시켜 화상을 형성하거나 전력을 생성하므로, 광을 투과시킬 수 있는 투명 도전막이 필수적이다. 이와 같은 투명 도전막으로는 인듐 주석 산화물(indium tin oxide, ITO)이 폭넓게 사용되고 있다. In general, a variety of electronic devices such as a display device, a light emitting diode, and a solar cell transmit light to form an image or generate electric power, so that a transparent conductive film capable of transmitting light is essential. As such a transparent conductive film, indium tin oxide (ITO) is widely used.
그러나 인듐 주석 산화물은 인듐의 소비량이 많아짐에 따라 가격이 높아져 경제성이 저하될 수 있으며, 특히 인듐을 포함하는 투명 도전막의 화학적, 전기적 결함이 존재하여 이를 대체할 수 있는 투명 도전 물질이 필요하다. However, as the consumption of indium tin oxide increases, the cost of indium tin oxide increases, leading to a decrease in cost efficiency. In particular, there is a need for a transparent conductive material capable of replacing the indium-containing transparent conductive film due to chemical and electrical defects.
이러한 투명 도전 물질로 그래핀(graphene)이 주목받고 있다. 그래핀은 복수 개의 탄소 원자들이 공유 결합으로 연결된 방향족 분자로, 약 10,000 내지 100,000 cm2/Vs의 높은 전자 이동도를 가질 뿐만 아니라 얇은 두께로 인하여 높은 광 투과도를 가진다. Graphene is drawing attention as such a transparent conductive material. Graphene is an aromatic molecule in which a plurality of carbon atoms are covalently linked to each other, and has high electron mobility of about 10,000 to 100,000 cm 2 / Vs as well as high light transmittance due to its thin thickness.
근래 그래핀으로 이루어진 그래핀 나노 리본(graphene nanoribbon)에 대한 연구가 이루어지고 있다. Recently, research on graphene nanoribbons made of graphene has been conducted.
상기 그래핀 나노 리본을 제조하는 방법으로 산화 환원 반응을 통해 탄소나노튜브(carbon nanotubes)의 옆면을 절개하고 펼치는 방법을 들 수 있다.As a method of manufacturing the graphene nano ribbon, a method of cutting and unfolding side surfaces of carbon nanotubes through a redox reaction may be mentioned.
그러나 상기 방법은 탄소나노튜브 자체를 사용함으로써 고가의 비용이 들고 산화 환원 반응 등 여러 단계가 필요하므로 공정이 복잡하고 제조 시간이 많이 걸린다. 뿐만 아니라, 산화 환원 반응 중에 그래핀 표면에 손상을 입힐 수 있고 하이드라진(hydrazine)과 같은 환경적으로 해로운 물질이 생성될 수 있다. 또한 상기 방법으로 제조된 나노 리본의 일부가 말려 있어서 이를 펴는데 추가적인 작업이 필요하다.
However, the method is expensive because of the use of carbon nanotubes itself and requires several steps such as a redox reaction, which makes the process complicated and takes a lot of manufacturing time. In addition, the graphene surface may be damaged during the redox reaction and environmentally harmful substances such as hydrazine may be produced. In addition, some of the nano-ribbon fabricated by the above method is curled, so additional work is required to straighten it.
일 구현예는 제조 공정을 단순화하고 제조 비용 및 시간을 줄일 수 있는 그래핀 나노 리본의 제조 방법을 제공한다.One embodiment provides a method of manufacturing a graphene nano ribbon that can simplify the manufacturing process and reduce manufacturing cost and time.
다른 구현예는 상기 방법으로 제조된 그래핀 나노 리본을 제공한다. Another embodiment provides a graphene nano ribbon prepared by the above method.
또 다른 구현예는 상기 그래핀 나노 리본을 포함하는 투명 도전막을 제공한다.Another embodiment provides a transparent conductive film including the graphene nano ribbon.
또 다른 구현예는 상기 투명 도전막을 포함하는 전자 소자를 제공한다.
Another embodiment provides an electronic device including the transparent conductive film.
일 구현예에 따르면, 구리 프탈로시아닌 및 이온성 액체를 포함하는 혼합물을 준비하는 단계, 그리고 상기 혼합물에 마이크로웨이브를 조사하는 단계를 포함하는 그래핀 나노 리본의 제조 방법을 제공한다.According to one embodiment, there is provided a method of preparing a graphene nano ribbon comprising preparing a mixture comprising copper phthalocyanine and an ionic liquid, and irradiating the mixture with microwaves.
상기 혼합물은 상기 구리 프탈로시아닌과 상기 이온성 액체가 약 1:0.5 내지 약 1:5의 중량비로 포함될 수 있다.The mixture may include the copper phthalocyanine and the ionic liquid in a weight ratio of about 1: 0.5 to about 1: 5.
상기 혼합물은 상기 구리 프탈로시아닌과 상기 이온성 액체가 약 1:1의 중량비로 포함될 수 있다.The mixture may include the copper phthalocyanine and the ionic liquid in a weight ratio of about 1: 1.
상기 이온성 액체는 1-에틸-3-메틸이미다졸륨(1-ethyl-3-methylimidazolium, EMIM)계 이온성 액체 및 1-부틸-3-메틸이미다졸륨(1-butyl-3-methylimidazolium, BMIM)계 이온성 액체 중 적어도 하나를 포함할 수 있다.The ionic liquid is a 1-ethyl-3-methylimidazolium (EMM) -based ionic liquid and 1-butyl-3-methylimidazolium (1-butyl-3-methylimidazolium, BMIM) based ionic liquids.
상기 1-에틸-3-메틸이미다졸륨(EMIM)계 이온성 액체는 1-에틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-ethyl-3-methylimidazolium tetrafluoroborate), 1-에틸-3-메틸이미다졸륨 헥사플루오로포스페이트(1-ethyl-3-methylimidazolium hexafluorophosphate), 1-에틸-3-메틸이미다졸륨 클로라이드(1-ethyl-3-methylimidazolium chloride), 1-에틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-ethyl-3-methylimidazolium trifluoroethane sulfonate), 1-에틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-ethyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)을 포함할 수 있다. The 1-ethyl-3-methylimidazolium (EMIM) -based ionic liquid is 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3- 1-ethyl-3-methylimidazolium hexafluorophosphate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimida 1-ethyl-3-methylimidazolium trifluoroethane sulfonate, 1-ethyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-ethyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide).
상기 1-부틸-3-메틸이미다졸륨(BMIM)계 이온성 액체는 1-부틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-butyl-3-methylimidazolium tetrafluoroborate), 1-부틸-3-메틸아미다졸륨 헥사플루오로포스페이트(1-butyl-3-methylimidazolium hexafluorophosphate), 1-부틸-3-메틸이미다졸륨 클로라이드(1-butyl-3-methylimidazolium chloride), 1-부틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-butyl-3-methylimidazolium trifluoroethane sulfonate), 1-부틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)를 포함할 수 있다.The 1-butyl-3-methylimidazolium (BMIM) -based ionic liquid is 1-butyl-3-methylimidazolium tetrafluoroborate (1-butyl-3-methylimidazolium tetrafluoroborate), 1-butyl-3- 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium chloride, 1-butyl-3-methylimida 1-butyl-3-methylimidazolium trifluoroethane sulfonate, 1-butyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-butyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide).
상기 혼합물에 마이크로웨이브를 조사하는 단계는 약 500 내지 1000W의 세기로 조사할 수 있다. Irradiating the microwave to the mixture may be irradiated with an intensity of about 500 to 1000W.
상기 혼합물에 마이크로웨이브를 조사하는 단계는 약 10 내지 300초 동안 조사할 수 있다. Irradiating the microwave to the mixture may be irradiated for about 10 to 300 seconds.
상기 혼합물에 마이크로웨이브를 조사하는 단계는 불연속적으로 수행할 수 있다.Irradiating the microwave to the mixture may be performed discontinuously.
상기 제조 방법은 상기 마이크로웨이브를 조사하는 단계 후에 상기 마이크로웨이브 조사된 혼합물 중에 흑색 성분을 추출하는 단계를 더 포함할 수 있다.The manufacturing method may further include extracting a black component in the microwave irradiated mixture after irradiating the microwave.
상기 제조 방법은 상기 흑색 성분을 추출하는 단계 후에 상기 흑색 성분을 초음파 처리하는 단계를 더 포함할 수 있다.The manufacturing method may further include the step of sonicating the black component after the step of extracting the black component.
상기 제조 방법은 상기 마이크로웨이브를 조사하는 단계 후에 상기 혼합물을 원심분리하여 미반응된 프탈로시아닌을 제거하는 단계를 더 포함할 수 있다.The method may further comprise the step of removing the unreacted phthalocyanine by centrifuging the mixture after the step of irradiating the microwave.
상기 제조 방법은 상기 마이크로웨이브를 조사하는 단계 후에 약 60 내지 120 ℃에서 건조하는 단계를 더 포함할 수 있다.The manufacturing method may further comprise the step of drying at about 60 to 120 ℃ after the step of irradiating the microwave.
다른 구현예에 따르면, 상술한 방법으로 제조된 그래핀 나노 리본을 제공한다.According to another embodiment, a graphene nano ribbon prepared by the above method is provided.
상기 그래핀 나노 리본은 끝이 말리지 않고 곧게 뻗은 형상을 가질 수 있다.The graphene nano ribbons may have a shape in which the ends thereof do not curl and extend straight.
또 다른 구현예는 상기 그래핀 나노 리본을 포함하는 투명 도전막을 제공한다.Another embodiment provides a transparent conductive film including the graphene nano ribbon.
또 다른 구현예는 상기 투명 도전막을 포함하는 전자 소자를 제공한다.
Another embodiment provides an electronic device including the transparent conductive film.
본 구현예에 따르면, 그래핀 나노 리본 제조시 공정을 단순화하고 제조 비용 및 시간을 줄일 수 있다. 또한 친환경적이고 경제적으로 다량의 나노 리본을 제조할 수 있다.
According to the present embodiment, it is possible to simplify the process in manufacturing the graphene nano ribbon and to reduce the manufacturing cost and time. In addition, eco-friendly and economically it is possible to manufacture a large amount of nanoribbons.
도 1은 실시예에 따른 그래핀 나노 리본의 주사전자현미경(scanning electron microscope, SEM) 사진이고,
도 2는 실시예에 따른 그래핀 나노 리본의 일정 부분을 확대한 주사전자현미경(SEM) 사진이고,
도 3은 실시예에 따른 그래핀 나노 리본을 에너지 분산형 X선 분석기(energy dispersive X-ray, EDX)로부터 나온 탄소 지도이고,
도 4는 실시예에 따른 그래핀 나노 리본의 투과전자현미경(transmission electron microscope, TEM) 사진이다.1 is a scanning electron microscope (SEM) photograph of a graphene nano ribbon according to an embodiment,
2 is a scanning electron microscope (SEM) photograph of a portion of a graphene nano ribbon according to an embodiment,
3 is a carbon map of the graphene nano ribbon according to an embodiment from an energy dispersive X-ray analyzer (EDX),
4 is a transmission electron microscope (TEM) photograph of the graphene nano ribbon according to the embodiment.
이하, 본 발명의 구현예에 대하여 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 상세히 설명한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며 여기에서 설명하는 구현예에 한정되지 않는다.Hereinafter, exemplary embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
일 구현예에 따른 그래핀 나노 리본의 제조 방법은 구리 프탈로시아닌(copper(II) phthalocyanine, CuPc) 및 이온성 액체를 포함하는 혼합물을 준비하는 단계, 그리고 상기 혼합물에 마이크로웨이브를 조사하는 단계를 포함한다.According to one or more exemplary embodiments, a method of preparing a graphene nano ribbon includes preparing a mixture including copper (II) phthalocyanine (CuPc) and an ionic liquid, and irradiating microwaves to the mixture. .
상기 혼합물은 상기 구리 프탈로시아닌과 상기 이온성 액체가 약 1:0.5 내지 약 1:5의 중량비로 포함될 수 있다. 상기 구리 프탈로시아닌과 상기 이온성 액체가 상기 비율로 포함됨으로써 후술하는 마이크로웨이브 조사 후 흑색 덩어리의 추출량을 충분히 확보할 수 있다. The mixture may include the copper phthalocyanine and the ionic liquid in a weight ratio of about 1: 0.5 to about 1: 5. Since the copper phthalocyanine and the ionic liquid are included in the above ratio, it is possible to sufficiently secure the extraction amount of the black mass after microwave irradiation described later.
상기 중량비 범위 내에서 상기 구리 프탈로시아닌과 상기 이온성 액체는 약 1:1의 중량비로 포함되는 것이 바람직하다.Within the weight ratio range, the copper phthalocyanine and the ionic liquid are preferably included in a weight ratio of about 1: 1.
상기 이온성 액체는 양이온과 음이온을 포함하는 이온성 염 화합물로, 상온에서 액체 상태로 존재할 수 있다. The ionic liquid is an ionic salt compound containing a cation and an anion, and may exist in a liquid state at room temperature.
상기 이온성 액체는 1-에틸-3-메틸이미다졸륨(1-ethyl-3-methylimidazolium, EMIM)계 이온성 액체 및/또는 1-부틸-3-메틸이미다졸륨(1-butyl-3-methylimidazolium, BMIM)계 이온성 액체를 포함할 수 있다.The ionic liquid is a 1-ethyl-3-methylimidazolium (EMI) based ionic liquid and / or 1-butyl-3-methylimidazolium (1-butyl-3- methylimidazolium (BMIM) based ionic liquids.
1-에틸-3-메틸이미다졸륨(EMIM)계 이온성 액체의 예로는 1-에틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-ethyl-3-methylimidazolium tetrafluoroborate), 1-에틸-3-메틸이미다졸륨 헥사플루오로포스페이트(1-ethyl-3-methylimidazolium hexafluorophosphate), 1-에틸-3-메틸이미다졸륨 클로라이드(1-ethyl-3-methylimidazolium chloride), 1-에틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-ethyl-3-methylimidazolium trifluoroethane sulfonate), 1-에틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-ethyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)을 들 수 있다.Examples of 1-ethyl-3-methylimidazolium (EMIM) -based ionic liquids include 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3 1-ethyl-3-methylimidazolium hexafluorophosphate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methyl Midazolium trifluoroethane sulfonate, 1-ethyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-ethyl-3- methylimidazolium bis [(trifluoromethyl) sulfonyl] imide).
1-부틸-3-메틸이미다졸륨(BMIM)계 이온성 액체의 예로는 1-부틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-butyl-3-methylimidazolium tetrafluoroborate), 1-부틸-3-메틸아미다졸륨 헥사플루오로포스페이트(1-butyl-3-methylimidazolium hexafluorophosphate), 1-부틸-3-메틸이미다졸륨 클로라이드(1-butyl-3-methylimidazolium chloride), 1-부틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-butyl-3-methylimidazolium trifluoroethane sulfonate), 1-부틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)을 들 수 있다.Examples of 1-butyl-3-methylimidazolium (BMIM) based ionic liquids include 1-butyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium chloride, 1-butyl-3-methyl Midazolium trifluoroethane sulfonate (1-butyl-3-methylimidazolium trifluoroethane sulfonate), 1-butyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-butyl-3- methylimidazolium bis [(trifluoromethyl) sulfonyl] imide).
상기 혼합물에 마이크로웨이브(microwave)를 조사하는 단계는 약 500 내지 1000W의 세기로 약 10 내지 300초 동안 수행될 수 있다. Irradiating the microwave to the mixture may be performed for about 10 to 300 seconds at an intensity of about 500 to 1000W.
이 때 상기 마이크로웨이브를 조사하는 단계는 불연속적으로 수행하는 것이 바람직하다. 즉 상기 혼합물에 마이크로웨이브를 약 5 내지 10 초 동안 조사한 후 잠시 공급을 끊었다가 잠시 후에 다시 조사하는 방식을 적어도 1회 이상 수행하는 것이 바람직하다. 이와 같이 마이크로웨이브 조사를 불연속적으로 수행함으로써 상기 혼합물이 타거나 스파크(spark)가 발생하는 것을 방지할 수 있다.At this time, the step of irradiating the microwave is preferably carried out discontinuously. That is, it is preferable to perform the method of irradiating the mixture for about 5 to 10 seconds and then temporarily discontinue the supply and irradiating again after a while at least one or more times. By discontinuously performing the microwave irradiation in this way it is possible to prevent the mixture from burning or sparking.
상기 혼합물에 마이크로웨이브를 조사하면, 상기 혼합물은 보라색 바탕에 흑색 덩어리들이 뭉쳐진 그래핀을 얻을 수 있다.When the mixture is irradiated with microwaves, the mixture may obtain graphene in which black lumps are aggregated on a purple background.
이어서 상기 혼합물 중에 흑색 성분만을 추출하고 상기 추출된 흑색 성분을 초음파 처리할 수 있다.Subsequently, only black components may be extracted from the mixture, and the extracted black components may be sonicated.
상기 초음파 처리는 예컨대 에틸알코올(ethyl alcohol)과 같은 알코올과 혼합한 후 초음파 배스(ultrasonic bath)에 넣어 수행할 수 있다. The sonication may be performed by mixing with an alcohol, such as ethyl alcohol, in an ultrasonic bath.
상기 초음파 처리하는 시간은 상기 추출된 흑색 성분의 양에 따라서 달라지며, 예컨대 약 15 내지 45 분 동안 수행할 수 있다. The sonication time depends on the amount of the extracted black component, for example, may be performed for about 15 to 45 minutes.
이어서 상기 초음파 처리된 혼합물을 약 10 내지 30분 동안 원심분리하여 미반응된 프탈로시아닌을 제거할 수 있다.The sonicated mixture may then be centrifuged for about 10 to 30 minutes to remove unreacted phthalocyanine.
마지막으로 상기 혼합물을 여과하고 건조하여 그래핀 나노 리본을 얻는다. 상기 건조 온도는 상기 초음파 처리에 사용된 용매의 종류에 따라 결정되며, 용매의 비점 이상의 온도에서 수행할 수 있다. 상기 건조 온도는 예컨대 약 60 내지 120 ℃일 수 있으며, 구체적으로는 용매가 알코올인 경우 약 80℃, 용매가 아세톤인 경우 약 60 내지 80℃, 용매가 디메틸포름알데히드(DMF)인 경우 약 120℃일 수 있다.Finally, the mixture is filtered and dried to obtain a graphene nano ribbon. The drying temperature is determined according to the type of the solvent used in the ultrasonic treatment, it can be carried out at a temperature above the boiling point of the solvent. For example, the drying temperature may be about 60 to 120 ° C., specifically about 80 ° C. when the solvent is alcohol, about 60 to 80 ° C. when the solvent is acetone, and about 120 ° C. when the solvent is dimethylformaldehyde (DMF). Can be.
상술한 방법은 별도의 산화 환원 반응이 필요하지 않으므로 제조 공정을 단순화하고 제조 시간을 줄일 수 있을 뿐만 아니라 친환경적이다. 따라서 다량의 그래핀 나노 리본을 제조할 수 있어서 경제적이다.Since the above-described method does not require a separate redox reaction, it is possible to simplify the manufacturing process and reduce the manufacturing time as well as to be environmentally friendly. Therefore, it is economical to manufacture a large amount of graphene nano ribbon.
상기 방법으로 제조된 그래핀 나노 리본은 끝이 말리지 않고 곧게 뻗은 형상을 가진다. 따라서 기존의 방법으로 나노 리본을 제조한 경우 나노 리본의 말린 부분을 펴기 위해 추가적인 작업이 필요한 것과 대비하여 공정을 더욱 단순화할 수 있다.The graphene nanoribbon prepared by the above method has a shape in which straight ends are not curled. Therefore, if the nanoribbons are manufactured by the conventional method, the process can be further simplified in case additional work is required to straighten the curled portions of the nanoribbons.
상기 그래핀 나노 리본의 두께는 나노미터 수준이며, 예컨대 약 0.1 내지 10nm 일 수 있다.The graphene nano ribbons have a thickness of about nanometers, for example, about 0.1 to about 10 nm.
상기 그래핀 나노 리본의 폭은 수십 내지 수백 나노미터일 수 있다.The width of the graphene nano ribbon may be several tens to hundreds of nanometers.
상기 그래핀 나노 리본은 우수한 전기적 특성, 즉 높은 전도도 및 낮은 접촉 저항을 가질 수 있고, 높은 광 투과도를 가질 수 있다. 따라서 다양한 전자 소자에서 투명 전극과 같은 투명 도전막으로 사용될 수 있으며, 경우에 따라 반도체로도 적용할 수 있다.The graphene nano ribbons may have excellent electrical properties, that is, high conductivity and low contact resistance, and may have high light transmittance. Therefore, it may be used as a transparent conductive film such as a transparent electrode in various electronic devices, and may be applied to a semiconductor in some cases.
상기 전자 소자는 투명 도전막을 포함하는 소자이면 한정되지 않으며, 예컨대 액정 표시 소자, 유기 발광 소자, 전자 종이 표시 소자, 태양 전지, 이미지 센서 등일 수 있다.
The electronic device is not limited as long as it includes a transparent conductive film, and may be, for example, a liquid crystal display device, an organic light emitting device, an electronic paper display device, a solar cell, an image sensor, or the like.
이하 실시예를 통하여 상술한 본 발명의 구현예를 보다 상세하게 설명한다. 다만 하기의 실시예는 단지 설명의 목적을 위한 것이며 본 발명의 범위를 제한하는 것은 아니다.
Hereinafter, embodiments of the present invention will be described in detail with reference to examples. The following examples are for illustrative purposes only and are not intended to limit the scope of the invention.
실시예Example
구리 프탈로시아닌과 1-에틸-3-메틸이미다졸륨 테트라플루오로보레이트(EMIM-BF4)을 1:1의 중량비로 혼합하였다. 이어서 상기 혼합물을 700W 마이크로웨이브 장치(Microwave Synthesis System, MAS-II)에 넣고 마이크로웨이브 장치를 온(on)하여 약 10 초 동안 마이크로웨이브를 조사하고 잠시 마이크로웨이브 장치를 오프(off) 한 후 다시 10 초 동안 마이크로웨이브 장치를 온(on)하였다. 이와 같이 마이크로웨이브 장치의 온/오프를 12 회 반복하여, 총 120초 동안 마이크로웨이브를 조사하였다. Copper phthalocyanine and 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIM-BF 4 ) were mixed in a weight ratio of 1: 1. Subsequently, the mixture was placed in a 700W microwave device (MAS-II), the microwave device was turned on, the microwave was irradiated for about 10 seconds, the microwave device was briefly turned off, and then again The microwave device was turned on for seconds. In this manner, the microwave device was repeatedly turned on and off 12 times, and the microwave was irradiated for 120 seconds in total.
이어서 마이크로웨이브 장치에서 혼합물을 꺼낸 후 흑색 덩어리 부분만 추출하고 이를 에틸알코올과 혼합하였다. 이어서 초음파 배스에 상기 혼합물을 넣고 30분간 초음파 처리하였다. 이어서 원심분리기를 사용하여 15분 동안 원심 분리를 수행한 후 여과하였다. 이어서 여과된 혼합물을 80℃에서 건조하여 그래핀 나노 리본을 얻었다.
Subsequently, the mixture was removed from the microwave apparatus, and only a black lump portion was extracted and mixed with ethyl alcohol. The mixture was then placed in an ultrasonic bath and sonicated for 30 minutes. Subsequent centrifugation was performed using a centrifuge for 15 minutes followed by filtration. The filtered mixture was then dried at 80 ° C. to obtain graphene nano ribbons.
그래핀Grapina 나노 리본의 확인 Confirmation of Nano Ribbon
상기 실시예에 따른 그래핀 나노 리본을 확인하였다.Graphene nano ribbon according to the embodiment was confirmed.
도 1은 실시예에 따른 그래핀 나노 리본의 주사전자현미경(scanning electron microscope, SEM) 사진이고, 도 2는 실시예에 따른 그래핀 나노 리본의 일정 부분을 확대한 주사전자현미경(SEM) 사진이고, 도 3은 실시예에 따른 그래핀 나노 리본을 에너지 분산형 X선 분석기(energy dispersive X-ray, EDX)로부터 나온 탄소 지도이고, 도 4는 실시예에 따른 그래핀 나노 리본의 투과전자현미경(transmission electron microscope, TEM) 사진이다.1 is a scanning electron microscope (SEM) photograph of a graphene nano ribbon according to an embodiment, and FIG. 2 is a scanning electron microscope (SEM) photograph of an enlarged portion of a graphene nano ribbon according to an embodiment. 3 is a carbon map of an graphene nano ribbon according to an embodiment from an energy dispersive X-ray analyzer (EDX), and FIG. 4 is a transmission electron microscope of the graphene nano ribbon according to an embodiment. transmission electron microscope (TEM).
도 1 및 도 2를 참고하면, 실시예에 따른 그래핀 나노 리본은 끝이 말리지 않고 곧게 뻗어 있는 형상을 가지는 것을 확인할 수 있다. 1 and 2, it can be seen that the graphene nano ribbon according to the embodiment has a shape in which the end is not straightened and extends straight.
도 3을 참고하면, 제조 결과물인 그래핀 나노 리본의 주요 성분이 탄소임을 확인할 수 있다. Referring to Figure 3, it can be seen that the main component of the graphene nano ribbons as a production result is carbon.
도 4를 참고하면, 실시예에 따른 그래핀 나노 리본은 투명한 것을 확인할 수 있다.Referring to Figure 4, it can be seen that the graphene nano ribbon according to the embodiment is transparent.
이로부터 실시예에 따른 그래핀 나노 리본은 끝이 말리지 않고 곧게 뻗은 형상을 가지면서도 충분히 투명한 것을 확인할 수 있다.
From this, it can be seen that the graphene nanoribbon according to the embodiment is sufficiently transparent while having a straight shape without curling its end.
이상에서 본 발명의 바람직한 실시예에 대하여 상세하게 설명하였지만 본 발명의 권리범위는 이에 한정되는 것은 아니고 다음의 청구범위에서 정의하고 있는 본 발명의 기본 개념을 이용한 당업자의 여러 변형 및 개량 형태 또한 본 발명의 권리범위에 속하는 것이다.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, Of the right.
Claims (16)
상기 혼합물에 마이크로웨이브를 조사하는 단계
를 포함하고,
상기 이온성 액체는 1-에틸-3-메틸이미다졸륨(1-ethyl-3-methylimidazolium, EMIM)계 이온성 액체 및 1-부틸-3-메틸이미다졸륨(1-butyl-3-methylimidazolium, BMIM)계 이온성 액체 중 적어도 하나를 포함하는
그래핀 나노 리본의 제조 방법.
Preparing a mixture comprising copper phthalocyanine and an ionic liquid, and
Irradiating microwaves to the mixture
Lt; / RTI >
The ionic liquid is a 1-ethyl-3-methylimidazolium (EMM) -based ionic liquid and 1-butyl-3-methylimidazolium (1-butyl-3-methylimidazolium, BMIM) based at least one of the ionic liquid
Method for producing graphene nano ribbons.
상기 혼합물은 상기 구리 프탈로시아닌과 상기 이온성 액체가 1:0.5 내지 1:5 의 중량비로 포함되어 있는 그래핀 나노 리본의 제조 방법.
In claim 1,
The mixture is a method for producing a graphene nano ribbon containing the copper phthalocyanine and the ionic liquid in a weight ratio of 1: 0.5 to 1: 5.
상기 혼합물은 상기 구리 프탈로시아닌과 상기 이온성 액체가 1:1의 중량비로 포함되어 있는 그래핀 나노 리본의 제조 방법.
3. The method of claim 2,
The mixture is a method for producing a graphene nano ribbon containing the copper phthalocyanine and the ionic liquid in a weight ratio of 1: 1.
상기 1-에틸-3-메틸이미다졸륨(EMIM)계 이온성 액체는 1-에틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-ethyl-3-methylimidazolium tetrafluoroborate), 1-에틸-3-메틸이미다졸륨 헥사플루오로포스페이트(1-ethyl-3-methylimidazolium hexafluorophosphate), 1-에틸-3-메틸이미다졸륨 클로라이드(1-ethyl-3-methylimidazolium chloride), 1-에틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-ethyl-3-methylimidazolium trifluoroethane sulfonate), 1-에틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-ethyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)을 포함하고,
상기 1-부틸-3-메틸이미다졸륨(BMIM)계 이온성 액체는 1-부틸-3-메틸이미다졸륨 테트라플루오로보레이트(1-butyl-3-methylimidazolium tetrafluoroborate), 1-부틸-3-메틸아미다졸륨 헥사플루오로포스페이트(1-butyl-3-methylimidazolium hexafluorophosphate), 1-부틸-3-메틸이미다졸륨 클로라이드(1-butyl-3-methylimidazolium chloride), 1-부틸-3-메틸이미다졸륨 트리플루오로에탄 설포네이트(1-butyl-3-methylimidazolium trifluoroethane sulfonate), 1-부틸-3-메틸이미다졸륨 비스[(트리플루오로메틸)설포닐]이미드(1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide)를 포함하는 그래핀 나노 리본의 제조 방법.
In claim 1,
The 1-ethyl-3-methylimidazolium (EMIM) -based ionic liquid is 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3- 1-ethyl-3-methylimidazolium hexafluorophosphate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimida 1-ethyl-3-methylimidazolium trifluoroethane sulfonate, 1-ethyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-ethyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide),
The 1-butyl-3-methylimidazolium (BMIM) -based ionic liquid is 1-butyl-3-methylimidazolium tetrafluoroborate (1-butyl-3-methylimidazolium tetrafluoroborate), 1-butyl-3- 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium chloride, 1-butyl-3-methylimida 1-butyl-3-methylimidazolium trifluoroethane sulfonate, 1-butyl-3-methylimidazolium bis [(trifluoromethyl) sulfonyl] imide (1-butyl-3-methylimidazolium A method for producing a graphene nano ribbon containing bis [(trifluoromethyl) sulfonyl] imide).
상기 혼합물에 마이크로웨이브를 조사하는 단계는 500 내지 1000W의 세기로 조사하는 그래핀 나노 리본의 제조 방법.
In claim 1,
Irradiating the microwave to the mixture is a method of producing a graphene nano ribbon to irradiate with an intensity of 500 to 1000W.
상기 혼합물에 마이크로웨이브를 조사하는 단계는 10 내지 300초 동안 조사하는 그래핀 나노 리본의 제조 방법.
The method of claim 6,
Irradiating the microwave to the mixture is a method of producing a graphene nano ribbon irradiated for 10 to 300 seconds.
상기 혼합물에 마이크로웨이브를 조사하는 단계는 불연속적으로 수행하는 그래핀 나노 리본의 제조 방법.
In claim 7,
Irradiating the microwave to the mixture is a method of producing a graphene nano ribbon is performed discontinuously.
상기 마이크로웨이브를 조사하는 단계 후에 상기 마이크로웨이브 조사된 혼합물 중에 흑색 성분을 추출하는 단계를 더 포함하는 그래핀 나노 리본의 제조 방법.
In claim 1,
And extracting a black component from the microwave irradiated mixture after the irradiating the microwaves.
상기 흑색 성분을 추출하는 단계 후에 상기 흑색 성분을 초음파 처리하는 단계를 더 포함하는 그래핀 나노 리본의 제조 방법.
The method of claim 9,
Method of producing a graphene nano ribbon further comprising the step of ultrasonicating the black component after the step of extracting the black component.
상기 흑색 성분을 초음파 처리하는 단계 후에 상기 혼합물을 원심분리하여 미반응된 프탈로시아닌을 제거하는 단계를 더 포함하는 그래핀 나노 리본의 제조 방법.
11. The method of claim 10,
The method of manufacturing a graphene nano ribbon further comprising the step of centrifuging the mixture after the step of sonicating the black component to remove unreacted phthalocyanine.
상기 마이크로웨이브를 조사하는 단계 후에 60 내지 120 ℃에서 건조하는 단계를 더 포함하는 그래핀 나노 리본의 제조 방법.
In claim 1,
Method of producing a graphene nano ribbon further comprising the step of drying at 60 to 120 ℃ after the step of irradiating the microwave.
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