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采用原位共生长化学气相沉积法, 以Co3O4、MoO3、Se粉末为前驱物, 710 ℃下在SiO2衬底上生长掺钴MoSe2纳米薄片, 分析讨论氢气含量对其生长及调节机理的影响. 表面形貌分析表明, 氢气的引入促进了成核所需的氧硒金属化合物以及横向生长中需要的CoMoSe化合物分子的生成; AFM(Atomic Force Microscope)结果表明氢气有利于生长单层二维超薄掺钴MoSe2. 随着Co3O4前驱物用量的增加, 样品的拉曼和PL(Photoluminescence)谱图分别表现出红移和蓝移现象, 带隙实现从1.52—1.57 eV的调制. XPS (X-ray photoelectron spectroscopy)结果分析得到Co的元素组分比为4.4%. 通过SQUID-VSM (Superconducting QUantum Interference Device)和器件电学测试分析了样品的磁电特性, 结果表明Co掺入后MoSe2由抗磁性变为软磁性; 背栅FETs器件的阈值电压比纯MoSe2向正向偏移5 V且关态电流更低; 为超薄二维材料磁电特性研究及应用拓展提供了基础探索.In this paper, Co3O4、MoO3 and Se powders were used as precursors in in-situ co-growth chemical vapor deposition method. Cobalt-doped MoSe2 nanosheets were grown on SiO2 substrate at 710 ℃. The influence of hydrogen content on its growth and regulation mechanism was discussed. Surface morphology analysis showed that the introduction of hydrogen promoted the formation of oxy-selenium metal compounds required for nucleation and the CoMoSe compound molecules required for lateral growth. AFM(atomic force microscope) results show that hydrogen is beneficial to the growth of single-layer two-dimensional cobalt-doped MoSe2. With the increase of the amount of Co3O4 precursor, the Raman and PL(photoluminescence) spectra of the sample showed red shift and blue shift, respectively, and the bandgap was modulated from 1.52 eV to 1.57 eV. The XPS(X-ray photoelectron spectroscopy) results analysis showed that the elemental composition ratio of Co was 4.4%. The magneto and electric properties of the samples were analyzed by SQUID-VSM(superconducting quantum interference device) and semiconductor parameter analyzer for electrical testing. The results show that MoSe2 changes from diamagnetic to soft magnetic after Co incorporation; the threshold voltage of back gate FETs is shifted by 5 V from pure MoSe2, and the off-state current is lower. This research provides a basis for the research and application development of ultra-thin two-dimensional materials.
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Keywords:
- two-dimensional materials /
- MoSe2 /
- Colbat-doping /
- chemistry phase deposition(CVD)
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图 1 化学气相沉积原位共生长掺钴MoSe2样品放置示意图
Fig. 1. Schematic illustration for Chemical vapor deposition in situ co-growth of cobalt-doped MoSe2.
图 2 不同氢气流量下生长掺Co MoSe2样品OM图
Fig. 2. OM of Co-doped MoSe2 under different H2 flow rates.
图 3 不同氢气流量下样品形貌情况 (a)−(d)为二维形貌图; (e)−(h)为沿红色虚线的高度测量结果
Fig. 3. Topographic measurements under different H2 flow rates: (a)−(d) Topography; (e)−(h) profile line along the red dash line.
图 4 (a)掺Co MoSe2的EDS谱图; (b)掺Co MoSe2样品EDS mapping图; (c)−(e)为未掺钴与掺钴的二硒化钼样品的XPS: (c) Co2p谱, (d) Mo3d谱和(e) Se3d谱
Fig. 4. (a) EDS spectrum of doped Co MoSe2; (b) EDS mapping of Co doped MoSe2; (c−e) XPS contrast spectra of MoSe2 and cobalt-doped MoSe2: (c) Co2p core level region, (d) Mo3d core level region and (e) Se3d core level region, respectively.
图 5 (a) MoSe2与掺Co MoSe2的拉曼图谱; (b)PL图谱; (c) MoSe2拉曼mapping图(238 cm–1); (d)掺Co MoSe2拉曼mapping图(235 cm–1)
Fig. 5. (a) Raman and (b) PL spectra of MoSe2 and Co-doped MoSe2; (c) raman mapping of MoSe2 (238 cm–1); (d) raman mapping Co-doped MoSe2 (235 cm–1).
图 6 (a) MoSe2与(b)不同Co3O4用量的掺Co MoSe2的VSM图
Fig. 6. VSM of (a) MoSe2 and (b) Co doped MoSe2 with different Co3O4 use level.
图 7 (a)未掺杂MoSe2与(b)掺Co MoSe2 FETs器件转移特性线性和对数坐标图
Fig. 7. Typical transfer characteristics of (a) undoped MoSe2 and (b) Co doped MoSe2 FETs device with semilog scale.
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[1] Larentis S, Fallahazad B, Tutuc E 2012 Appl. Phys. Lett. 101 223104
Google Scholar
[2] Wang Q H, Kalantar-Zadeh K, Kis A, Coleman J N, Strano M S 2012 Nat. Nanotechnol. 7 699
Google Scholar
[3] Li Y, Zhang K, Wang F, Feng Y, Li Y, Han Y, Tang D, Zhang B 2017 ACS Appl. Mater. Interfaces. 9 36009
Google Scholar
[4] Li X, Puretzky A A, Sang X, KC S, Tian M, Ceballos F, Mahjouri‐Samani M, Wang K, Unocic R R, Zhao H 2017 Adv. Funct. Mater. 27 1603850
Google Scholar
[5] Huang B, Yoon M, Sumpter B G, Wei S-H, Liu F 2015 Appl. Phys. Lett. 115 126806
Google Scholar
[6] Fan S, Shen W, An C, Sun Z, Wu S, Xu L, Sun D, Hu X, Zhang D, Liu J 2018 ACS Appl. Mater. Interfaces. 10 26533
Google Scholar
[7] Feng Q, Mao N, Wu J, Xu H, Wang C, Zhang J, Xie L 2015 ACS Nano. 9 7450
Google Scholar
[8] Feng Q, Zhu Y, Hong J, Zhang M, Duan W, Mao N, Wu J, Xu H, Dong F, Lin F, Jin C, Wang C, Zhang J, Xie L 2014 Adv. Mater. 26 2648
Google Scholar
[9] Tang D, Wang F, Zhang B, Li Y, Li Y, Feng Y, Han Y, Ma J, Ren T, and Zhang K 2018 J. Mater. Sci. 53 14447
Google Scholar
[10] Li X, Lin M W, Basile L, Hus S M, Puretzky A A, Lee J, Kuo Y C, Chang L Y, Wang K, Idrobo J C, Li A P, Chen C-H, Rouleau C M, Geohegan D B, Xiao K 2016 Adv. Mater. 28 8240
Google Scholar
[11] Cheng Y C, Zhu Z, Mi W B, Guo Z B, Schwingenschlögl U 2013 Phys. Rev. B. 87 100401
Google Scholar
[12] Xie L Y, Zhang J M 2016 Superlattices Microstruct. 98 148
[13] Xu R, Liu B, Zou X, Cheng H M 2017 ACS Appl. Mater. Interfaces. 9 38796
Google Scholar
[14] Li B, Huang L, Zhong M, Huo N, Li Y, Yang S, Fan C, Yang J, Hu W, Wei Z, Li J 2015 ACS Nano. 9 1257
Google Scholar
[15] Chen X, Qiu Y, Liu G, Zheng W, Feng W, Gao F, Cao W, Fu Y, Hu W, Hu P 2017 J. Mater. Chem. A. 5 11357
Google Scholar
[16] 黄静雯, 罗利琼, 金波, 楚士晋, 彭汝芳 2017 66 137801
Google Scholar
Huang J W, Luo L Q, Jin B, Chu S J, Peng R F 2017 Acta Phys. Sin. 66 137801
Google Scholar
[17] Zhang J, Yu H, Chen W, Tian X, Liu D, Cheng M, Xie G, Yang W, Yang R, Bai X, Shi D, Zhang G 2014 ACS nano. 8 6024
Google Scholar
[18] Tu Z, Li G, Ni X, Meng L, Bai S, Chen X, Lou J, Qin Y 2016 Appl. Phys. Lett. 109 223101
Google Scholar
[19] Rong Y, Fan Y, Koh A L, Robertson A W, He K, Wang S, Tan H, Sinclair R, Warner J H 2014 Nanoscale. 6 12096
Google Scholar
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Google Scholar
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Google Scholar
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Google Scholar
[23] Cheng J, Jiang T, Ji Q, Zhang Y, Li Z, Shan Y, Zhang Y, Gong X, Liu W, Wu S 2015 Adv. Mater. 27 4069
Google Scholar
[24] Gao Y, Hong Y L, Yin L C, Wu Z, Yang Z, Chen M L, Liu Z, Ma T, Sun D M, Ni Z, Ma X-L, Cheng H-M, Ren W 2017 Adv. Mater. 29 1700990
Google Scholar
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