KR101691196B1 - 질소 도핑된 그래핀의 제조방법 및 이로부터 제조된 질소 도핑된 그래핀 - Google Patents
질소 도핑된 그래핀의 제조방법 및 이로부터 제조된 질소 도핑된 그래핀 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
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- Engineering & Computer Science (AREA)
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Abstract
Description
도 2는 본 발명의 일 실시예에 따른 N-MLG-45min의 (a) TEM 이미지, (b) AFM 이미지, (c) XPS 그래프, (d) 라만 스펙트럼을 나타낸 것이다.
도 3은 본 발명의 일 실시예에 따른 XPS 그래프를 나타낸 것이다. ((a) N-MLG-45min의 질소에 대한 XPS 그래프, (b) N-MLG-45min, N-MLG-90min, N-MLG-120min의 질소에 대한 XPS 그래프)
도 4는 본 발명의 N-MLG-45min, N-MLG-90min, N-MLG-120min의 라만 스펙트럼을 나타낸 것이다.
도 5는 본 발명의 일 실시예에 따른 (a) 선형 주사 전압-전류곡선, (b) 회전 원판 전압-전류곡선, (c) Koutecky-Levich 그래프, (d) Fe함량에 따른, 선형 주사 전압-전류 곡선을 나타낸 것이다.
도 6은 본 발명의 실시예 1 내지 실시예 3에 따른 TGA 곡선을 나타낸 것이다.
N-MLG-45min | N-MLG-90min | N-MLG-120min | |
Fe기판제조단계 열처리(1000℃) 반응시간(min) |
45 | 90 | 120 |
실시예 1 | 실시예 2 | 실시예 3 | 실시예 4 | 실시예 5 | 실시예 6 | 실시예 7 | |
Fe기판제조단계 열처리(1000℃) 반응시간(min) |
45 | 60 | 90 | ||||
Fe제거반응 (HCl 처리시간) |
0 | 3 | 6 | 0 | 6 | 0 | 6 |
시료 | 총질소(N)함량 (at.%) | XPS 분석(%) | 결합 에너지(eV) | ||||
N | N1 | N2 | N3 | N1 | N2 | N3 | |
N-MLG-45min | 7.41 | 34.6 | 30.6 | 34.8 | 398.7 | 400.3 | 402.0 |
N-MLG-90min | 6.13 | 30.4 | 29.9 | 39.7 | |||
N-MLG-120min | 3.45 | 24.8 | 30.1 | 45.1 |
시료 | XPS 분석(at.%) | |||
C | N | Fe | O | |
실시예 1 | 62.30 | 4.97 | 26.45 | 6.28 |
실시예 3 | 79.88 | 7.41 | - | 12.71 |
실시예 4 | 63.80 | 3.54 | 26.42 | 6.24 |
실시예 5 | 83.25 | 6.13 | - | 10.62 |
실시예 6 | 67.63 | 2.48 | 26.75 | 3.14 |
실시예 7 | 87.82 | 3.45 | - | 8.73 |
Claims (11)
- 밀크파우더 및 멜라민을 8~9.6 : 1의 중량비로 산성용액에 투입하여 가열 및 교반하여 열분해함으로써 탄소원자 및 질소원자를 포함하는 혼합물 용액을 제조하는 제 1 단계;
상기 혼합물 용액에 암모늄 기를 더 포함하는 Fe2+이온을 포함하는 용액을 첨가하여 교반하는 제 2 단계;
상기 제 2 단계 후, 질소 분위기 하에서 850~1200℃에서 45~90분 동안 열처리함으로써, Fe 기판을 형성하는 제 3 단계;
상기 제 3 단계를 거친 후, 냉각시킴으로써 상기 탄소원자 및 질소원자를 상기 Fe 기판 상에 확산하여 질소가 도핑된 다층 그래핀을 형성하는 제 4 단계; 및
상기 제 4 단계를 거친 후, 상기 Fe 기판을 제거하는 제 5 단계;를 포함하고,
상기 질소가 도핑된 다층 그래핀은, 전체 중량 100%에 대해 피리딘 유사배열, 피롤 유사배열 및 그라파이트 유사배열로 이루어진 6.0~7.41중량%의 도핑된 질소를 포함하고, 상기 피리딘 유사배열 질소는 상기 도핑된 질소 중량 100%에 대해 30~35중량%로 포함되는 것을 특징으로 하는, 밀크파우더 및 멜라민을 이용하는 질소가 도핑된 다층 그래핀의 제조방법. - 제 1 항에 있어서,
상기 제 5 단계는, 상기 제 4 단계를 거친 후 산을 첨가하여 80℃에서 6시간 동안 반응시킴으로써 Fe기판을 제거하는 것을 특징으로 하는, 밀크파우더 및 멜라민을 이용하는 질소가 도핑된 다층 그래핀의 제조방법. - 삭제
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KR1020140123501A KR101691196B1 (ko) | 2014-09-17 | 2014-09-17 | 질소 도핑된 그래핀의 제조방법 및 이로부터 제조된 질소 도핑된 그래핀 |
PCT/KR2015/003464 WO2016043396A1 (ko) | 2014-09-17 | 2015-04-07 | 질소 도핑된 그래핀의 제조방법 및 이로부터 제조된 질소 도핑된 그래핀 |
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KR101691196B1 true KR101691196B1 (ko) | 2016-12-30 |
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TR201819187A2 (tr) * | 2018-12-12 | 2020-06-22 | Yueksel Yenilenebilir Enerji Anonim Sirketi | Azot katkılanmış grafen üretimi yöntemi. |
KR102216959B1 (ko) * | 2019-05-13 | 2021-02-18 | 한국전력공사 | 그래핀 제조용 조성물, 이를 이용한 그래핀 제조 방법 및 그래핀 |
KR102509798B1 (ko) * | 2021-04-20 | 2023-03-14 | 고려대학교 산학협력단 | 전이금속 칼코겐 화합물 도핑 방법 |
KR102603475B1 (ko) * | 2021-07-29 | 2023-11-16 | 인하대학교 산학협력단 | 질소 도핑된 흑연 나노 구조체의 제조방법 및 응용 |
CN115957790B (zh) * | 2022-08-18 | 2024-09-03 | 温州大学 | 一种氮掺杂石墨烯三维宏观体催化剂及其制备方法 |
WO2025009914A1 (ko) * | 2023-07-04 | 2025-01-09 | 서울대학교산학협력단 | 도핑된 그래파이트 플레이크의 제조방법 |
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