激光冲击法合成纳米金刚石的研究
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摘要
为了提高激光冲击法合成纳米金刚石的效率,本文首次提出激光照射循环水介质中石墨颗粒合成纳米金刚石的新工艺,并对激光冲击法合成纳米金刚石的工艺和理论进行了研究。采用高分辨透射电镜、扫描电镜、能谱仪、X射线衍射仪和显微激光拉曼光谱仪等手段进行分析,发现本实验条件下合成的纳米金刚石颗粒尺寸约为5nm,具有球形单晶体结构或五重孪晶结构。本课题进行了以下研究:
(1)从粒度、石墨化程度以及各种原料中六方石墨和菱方石墨的相对含量方面对原料组织结构进行了详细的分析;
(2)研究不同激光器对合成纳米金刚石的影响。试验中,以石墨为原料,分别采用Nd:YAG毫秒脉冲激光器、红宝石Q开关纳秒脉冲激光器和CO2连续激光器三种不同模式、不同功率密度激光器,成功地合成了纳米金刚石;
(3)根据实验结果和前人的工作基础,认为功率密度≥109 W·cm~(-2)的激光照射石墨悬浮液时,其相变机理为:在石墨颗粒表面产生高温高压高密度的碳等离子体,在随后的冷却过程中形成纳米金刚石;
(4)根据透射电镜对纳米金刚石的组织结构分析结果,认为功率密度在10~5～10~6W·cm~(-2)范围的激光照射石墨悬浮液时,不能产生等离子体,其相变机理为:石墨颗粒吸收激光能量时快速升温并达到熔融状态,激光脉冲过后,碳液滴迅速冷却,金刚石形核并长大;
(4)实验研究发现,纳米金刚石粉末的热稳定性低于石墨和炭黑粉末,在相同温度下,纳米金刚石比石墨和炭黑粉末更容易氧化,因此不能用这种简单的热氧化方法来提纯纳米金刚石;
(5)根据实验结果,讨论了不同石墨原料、不同激光对合成纳米金刚石的影响,认为在高功率密度(≥109 W·cm~(-2))激光情况下,粗颗粒石墨原料对合成纳米金刚石有利;而对功率密度在10~5～10~6W·cm~(-2)范围,细颗粒石墨原料对合成纳米金刚石有利;
(6)开展理论研究,包括激光与材料相互作用物理学、纳米金刚石颗粒尺寸限制的机制、碳的状态方程以及金刚石临界形核半径的估算等。本课题的主要创新点为:(1)首次提出激光照射循环的石墨悬浮液合成纳米金刚石的新工艺;(2)首次在较低功率密度(10~5～10~6W·cm~(-2))激光用石墨成功合成出纳米金刚石;(3)首次提出了低功率密度激光合成纳米金刚石的转变模型;(4)首次研究不同石墨原料对合成纳米金刚石的影响。
In order to improve the transformation ratio of nanodiamond synthesized by laser irradiation, in this research, we proposed the process that the graphite particles suspended in water was irradiated by laser beam for the first time. The mechanism of phase transformation in the synthesis was investigated from the aspects of experimental process and theoretical analysis.
High resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) X-ray diffract meter (XRD) and micro-Raman spectroscopy were used to invetigate the synthesis of nanodiamonds. The results suggest that diamond particles with monocrystal structure or multiple twins’structure be synthesized and the particles size be about 5 nm in the samples. The details are shown as follows:
(1) The raw materials’particle size, degree of graphitization and the ratio of hexagonal and rhombohedral graphite were analyzed.
(2) Nanodiamonds are synthesized sucessfully when the graphite powders were irradiated by pulsed Nd:YAG laser, pulsed ruby laser or continuous CO2 .
(3) The mechanism of the phase transformation in the process was presented. For the laser beam with high power density (≥109 W·cm~(-2)), high temperature, high pressure and high density carbon plasma was generated when laser irradiated the graphite powders, then nanodimonds formed during the cooling process.
(4) For the laser beam with power density (10~5～10~6W·cm~(-2)) which can not generate plasma, the raw graphite was molten, and nanodiamond nucleated and grew up from liquid carbon cooled quickly.
(5)According to the experimental results, the raw material with samller particle size is favorable to the synthesis of nanodiamond for the laser beam with power density(10~5～10~6W·cm~(-2)) and the coarser particle for the laser beam with high power density(≥109 W·cm~(-2)).
(6)The physics of laser beam interacting with materials and several equation for carbon at different structure and state, such as graphite, diamond and liquid carbon, have been introduced. An evaluation of equilibrium state and critical size of nanodiamond is also presented.
The novelties of the research: 1) The process that the graphite particles suspended in water was irradiated by laser beam was proposed for the first time. 2) Nanodiamonds are synthesized under the power density as low as 105 W·cm~(-2) for the first time. 3)The suspending liquid is circulated to attain continuous synthesis; 4) The graphite particles are used as the target to improve the conversion ratio of nanodiamond;
(1)从粒度、石墨化程度以及各种原料中六方石墨和菱方石墨的相对含量方面对原料组织结构进行了详细的分析;
(2)研究不同激光器对合成纳米金刚石的影响。试验中,以石墨为原料,分别采用Nd:YAG毫秒脉冲激光器、红宝石Q开关纳秒脉冲激光器和CO2连续激光器三种不同模式、不同功率密度激光器,成功地合成了纳米金刚石;
(3)根据实验结果和前人的工作基础,认为功率密度≥109 W·cm~(-2)的激光照射石墨悬浮液时,其相变机理为:在石墨颗粒表面产生高温高压高密度的碳等离子体,在随后的冷却过程中形成纳米金刚石;
(4)根据透射电镜对纳米金刚石的组织结构分析结果,认为功率密度在10~5～10~6W·cm~(-2)范围的激光照射石墨悬浮液时,不能产生等离子体,其相变机理为:石墨颗粒吸收激光能量时快速升温并达到熔融状态,激光脉冲过后,碳液滴迅速冷却,金刚石形核并长大;
(4)实验研究发现,纳米金刚石粉末的热稳定性低于石墨和炭黑粉末,在相同温度下,纳米金刚石比石墨和炭黑粉末更容易氧化,因此不能用这种简单的热氧化方法来提纯纳米金刚石;
(5)根据实验结果,讨论了不同石墨原料、不同激光对合成纳米金刚石的影响,认为在高功率密度(≥109 W·cm~(-2))激光情况下,粗颗粒石墨原料对合成纳米金刚石有利;而对功率密度在10~5～10~6W·cm~(-2)范围,细颗粒石墨原料对合成纳米金刚石有利;
(6)开展理论研究,包括激光与材料相互作用物理学、纳米金刚石颗粒尺寸限制的机制、碳的状态方程以及金刚石临界形核半径的估算等。本课题的主要创新点为:(1)首次提出激光照射循环的石墨悬浮液合成纳米金刚石的新工艺;(2)首次在较低功率密度(10~5～10~6W·cm~(-2))激光用石墨成功合成出纳米金刚石;(3)首次提出了低功率密度激光合成纳米金刚石的转变模型;(4)首次研究不同石墨原料对合成纳米金刚石的影响。
In order to improve the transformation ratio of nanodiamond synthesized by laser irradiation, in this research, we proposed the process that the graphite particles suspended in water was irradiated by laser beam for the first time. The mechanism of phase transformation in the synthesis was investigated from the aspects of experimental process and theoretical analysis.
High resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) X-ray diffract meter (XRD) and micro-Raman spectroscopy were used to invetigate the synthesis of nanodiamonds. The results suggest that diamond particles with monocrystal structure or multiple twins’structure be synthesized and the particles size be about 5 nm in the samples. The details are shown as follows:
(1) The raw materials’particle size, degree of graphitization and the ratio of hexagonal and rhombohedral graphite were analyzed.
(2) Nanodiamonds are synthesized sucessfully when the graphite powders were irradiated by pulsed Nd:YAG laser, pulsed ruby laser or continuous CO2 .
(3) The mechanism of the phase transformation in the process was presented. For the laser beam with high power density (≥109 W·cm~(-2)), high temperature, high pressure and high density carbon plasma was generated when laser irradiated the graphite powders, then nanodimonds formed during the cooling process.
(4) For the laser beam with power density (10~5～10~6W·cm~(-2)) which can not generate plasma, the raw graphite was molten, and nanodiamond nucleated and grew up from liquid carbon cooled quickly.
(5)According to the experimental results, the raw material with samller particle size is favorable to the synthesis of nanodiamond for the laser beam with power density(10~5～10~6W·cm~(-2)) and the coarser particle for the laser beam with high power density(≥109 W·cm~(-2)).
(6)The physics of laser beam interacting with materials and several equation for carbon at different structure and state, such as graphite, diamond and liquid carbon, have been introduced. An evaluation of equilibrium state and critical size of nanodiamond is also presented.
The novelties of the research: 1) The process that the graphite particles suspended in water was irradiated by laser beam was proposed for the first time. 2) Nanodiamonds are synthesized under the power density as low as 105 W·cm~(-2) for the first time. 3)The suspending liquid is circulated to attain continuous synthesis; 4) The graphite particles are used as the target to improve the conversion ratio of nanodiamond;
引文
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