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Chin. Phys. B, 2020, Vol. 29(10): 108102    DOI: 10.1088/1674-1056/abad1c
INTERDISCIPLINARY PHYSICS AND RELATED AREAS OF SCIENCE AND TECHNOLOGY Prev   Next  

Two-step high-pressure high-temperature synthesis of nanodiamonds from naphthalene

Tong Liu(刘童)1, Xi-Gui Yang(杨西贵)1,†(), Zhen Li(李振)1, Yan-Wei Hu(胡宴伟)1, Chao-Fan Lv(吕超凡)1, Wen-Bo Zhao(赵文博)1, Jin-Hao Zang(臧金浩)1,‡(), Chong-Xin Shan(单崇新)1,§
1 Henan Key Laboratory of Diamond Optoelectronic Materials and Devices, Key Laboratory of Materials Physics, Ministry of Education, School of Physics and Microelectronics, Zhengzhou University, Zhengzhou 450052, China
Abstract  

Nanodiamonds have outstanding mechanical properties, chemical inertness, and biocompatibility, which give them potential in various applications. Current methods for preparing nanodiamonds often lead to products with impurities and uneven morphologies. We report a two-step high-pressure high-temperature (HPHT) method to synthesize nanodiamonds using naphthalene as the precursor without metal catalysts. The grain size of the diamonds decreases with increasing carbonization time (at constant pressure and temperature of 11.5 GPa and 700 °C, respectively). This is discussed in terms of the different crystallinities of the carbon intermediates. The probability of secondary anvil cracking during the HPHT process is also reduced. These results indicate that the two-step method is efficient for synthesizing nanodiamonds, and that it is applicable to other organic precursors.

Keywords:  nanodiamonds      high pressure high temperature      phase transition      naphthalene  
Received:  25 July 2020      Revised:  03 August 2020      Published:  05 October 2020
PACS:  81.05.ug (Diamond)  
  62.50.-p (High-pressure effects in solids and liquids)  
  64.70.Nd (Structural transitions in nanoscale materials)  
  07.35.+k (High-pressure apparatus; shock tubes; diamond anvil cells)  
Corresponding Authors:  Corresponding author. E-mail: yangxg@zzu.edu.cn Corresponding author. E-mail: jinhao_zang@zzu.edu.cn §Corresponding author. E-mail: cxshan@zzu.edu.cn   
About author: 
†Corresponding author. E-mail: yangxg@zzu.edu.cn
‡Corresponding author. E-mail: jinhao_zang@zzu.edu.cn
§Corresponding author. E-mail: cxshan@zzu.edu.cn
* Project supported by the National Key R&D Program of China (Grant No. 2018YFB0406500), the National Natural Science Foundation of China (Grant Nos. U1804155, U1604263, and 11804307), and the China Postdoctoral Science Foundation (Grant Nos. 2018M630830 and 2019T120631).

Cite this article: 

Tong Liu(刘童), Xi-Gui Yang(杨西贵), Zhen Li(李振), Yan-Wei Hu(胡宴伟), Chao-Fan Lv(吕超凡), Wen-Bo Zhao(赵文博), Jin-Hao Zang(臧金浩), Chong-Xin Shan(单崇新) Two-step high-pressure high-temperature synthesis of nanodiamonds from naphthalene 2020 Chin. Phys. B 29 108102

Scheme 1.  

Schematic of the synthesis of nanodiamonds via the two-step HPHT method. 1. cylindrical sample of the precursor naphthalene; 2. graphite container; 3. ZrO2 sleeve; 4. octahedron pressure medium of MgO.

Fig. 1.  

(a) XRD patterns and (b) Raman spectra of the naphthalene precursor and samples NX (X = 1–4) prepared using different carbonization time at 11.5 GPa and 1700 °C.

Step 1: Carbonization at 11.5 GPa and 700 °C Step 2: Diamondation at 11.5 GPa and 1700 °C
Timea/min Morphology Timeb/s Average size/nm
N1 35 / 300 457
N2 90 / 300 204
N3 135 / 300 62
N4 180 / 300 127
N5 35 amorphous / /
N6 90 chipped / /
N7 135 layered / /
N8 180 block / /
Table 1.  

The experimental conditions and results for samples NX (X = 1–8).

Fig. 2.  

(a)–(d) Grain size distributions of samples NX (X = 1–4) prepared using different carbonization time. The red curves show fitting of the lognormal distribution function. Inset shows the corresponding SEM images.

Fig. 3.  

Average grain size of samples NX (X = 1–4) as a function of carbonization time.

Fig. 4.  

(a) TEM image of sample N3. Inset shows HRTEM image of a single diamond particle from the white rectangle area marked in (a). (b) Selected area electron diffraction pattern of sample N3.

Fig. 5.  

(a) XRD patterns, (b) Raman spectra, and (c)–(f) SEM images of samples NX (X = 5–8) obtained using different carbonization time at 11.5 GPa and 700 °C.

Fig. 6.  

Raman spectra of diamond obtained employing (a) anthracene and (b) acridine as precursors in the two-step HPHT method.

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