碳包覆金属纳米粒子制备与应用基础研究
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摘要
碳包覆金属纳米粒子(Carbon Encapsulated Metal Nano-Particles，CEMNPs)是一种具有核/壳结构的金属/碳纳米复合材料。多种金属纳米材料内核与碳壳的不同组合赋予这种复合材料众多奇特的物理化学性能，在生物医学、化工、新能源等许多领域都显示出巨大的潜在应用前景，比如作为磁共振成像造影剂、生物分析和药物载体、高热疗法介质、催化剂、磁记录和磁分离介质等。作为一种新型的碳复合纳米材料，碳包覆金属纳米粒子的制备、性质及应用基础研究已成为广泛关注的热点。人们已用多种方法合成不同金属粒子的纳米碳包覆材料。目前，主要的制备方法包括高能生长法（电弧、离子束、激光、爆炸）和化学气相沉积、碳基转化等等，能耗高、设备要求高、制备工艺复杂、价格昂贵。碳包覆金属纳米粒子，特别是核为磁性金属的CEMNPs，生产效率较低，制约了关于CEMNPs的应用基础研究发展。
本文以价格低廉、获取方便的蔗糖和金属硝酸盐为主要原料，首先采用热解法在N2气氛下制备出碳包覆钴纳米粒子(记为Co@C)、碳包覆铜镍纳米粒子(记为CuNi@C)；在此基础上，将软化学方法和热解法与结合，提出了液相还原-高温炭化法，制备出碳包覆铜纳米粒子(记为Cu@C)、碳包覆铁纳米粒子(记为Fe@C)、碳包覆钴纳米粒子[记为Co@C(LR)]和碳包覆铁铜纳米粒子(记为FeCu_4@C)，实现了CEMNPs成单分散状。对所制备的CEMNPs，采用多种现代分析测试方法对其化学组成、物相、显微结构和一些主要物理、化学性质进行了较为系统的表征，试验研究了碳包覆金属纳米粒子作为润滑油添加剂对摩擦磨损性能的影响；探讨了碳包覆金属纳米粒子修饰玻碳电极的电化学催化性能。研究结果表明：
Co@C的核为fcc-Co、壳为多层同心层状六角形碳网，在碳网上连接有=O、-OH等基团。在Co@C纳米粒子外围存在无定形碳，分散粒径均值162.8nm， TEM测定粒径均值35.3nm。室温下其饱和磁化强度M_s=24.7emu/g，剩余磁化强度M_r=3.71emu/g，矫顽力H_c=275.2Oe。碳壳保护作用明显，金属核在1000℃后才氧化。Co@C具有一定的导电性，常温电阻率9.46·cm。对于8～18GHz微波具有一定的吸收能力，在14.7GHz时吸收最大为6.36dB。
Co@C(LR)壳层为无定形碳，核为多晶fcc-Co，基本呈单分散状，平均粒径49.6nm。样品中不足1/5的碳为纯C-C结合，其余均连接有其它基团，钴核主要呈现0价金属态和少量氧化态。室温下Co@C(LR)的M_s=130.7emu/g、M_r=13.0emu/g，H_c=56Oe，表现出超顺磁性。BET法测试的Co@C(LR)比表面积SSA=167.0m2/g。在液体石蜡中添加Co@C进行的摩擦磨损试验发现：当添加量为0.6wt%时其承载力有所提高，添加量为0.4wt%时摩擦系数μ和磨痕宽度W最小，均低于对照油，说明Co@C(LR)有一定的减摩抗磨效果。对比以裸玻碳电极(GCE)和以Co@C(LR)修饰的GCE为工作电极时得到的CV曲线，Co@C(LR)对对硝基苯酚(PNP)的电化学反应有良好的催化效果。
CuNi@C的核为多晶fcc-CuNi合金，壳为可观察到石墨结构层的C，但晶格条纹不够连续、完整。壳外粘连有无定形碳，其分散粒径为134.1nm、TEM测试粒径为55nm。样品中约1/3的碳为纯C-C结合，余下的都与其它基团有相互作用，Cu、Ni都存在金属态和氧化态两种形式。CuNi@C有一定的导电性，室温电阻率为100.56Ω cm，对于8～18GHz微波具有一定的吸收能力，在14.9GHz时吸收最大为8.1dB。将CuNi@C添加到液体石蜡中进行的摩擦磨损试验结果表明，当添加量为0.6wt%时有效降低了摩擦系数μ和磨痕宽度W，表现出了较好的减摩抗磨性能。
Fe@C的核主要是多晶bcc-Fe，壳为无定形碳，为单分散状，平均粒径48nm。样品中约43%的碳为C-C结合，其余与其-OH、-N有相互作用，约76%的Fe为0价金属，其余为Fe~(3+)。磁性能测试结果为：M_s=54.56emu/g，M_r=5.35emu/g， H_c=205Oe。BET法测得的SSA=522.7m~2/g。Fe@C对PNP的电化学反应有良好的催化效果，最佳NaOH浓度为1mol/L。
Cu@C的核为多晶fcc-Cu，壳为无定形碳，局部能观察到晶格条纹，单分散状，平均粒径49.5nm。约1/2的C为纯C-C连接，其余的连接有其它基团，Cu有0价金属和CuO两种状态。BET法测得的SSA=94.1m~2/g。在液体石蜡中添加一定量的Cu@C具有明显的减摩抗磨效果，当添加量为0.6wt%时，与对照油相比μ降低了21.6%，W降低了30.0%。Cu@C对PNP的电化学反应有良好的催化效果，最佳NaOH浓度为0.5mol/L。
FeCu_4@C的核为fcc-FeCu_4，壳为无定形碳，单分散状，平均粒径62.8nm。约36%的C为纯C-C连接，其余的连接有其它基团，Cu有0价金属和Cu(OH)_2两种状态，Fe含量低，只检测到0价金属态。磁性能测试结果为：M_s=13.01emu/g，M_r=0.37emu/g，H_c=54.43Oe。BET法测得的SSA=269.9m~2/g。
基于上述研究工作在碳包覆金属纳米粒子制备方法、性能表征和摩擦学性能研究等方面获得的知识，丰富了碳包覆金属纳米材料的基础理论，在促进应用技术发展方面提供了支持。
Carbon encapsulated metal nano-particles (CEMNPs)are types of carbon/metalcomposite materials with core/shell structure in nanoscale. The different combination ofvarious metal nanometer materials as core and carbon as shell rewards the composite withmany peculiar physical and chemical properties.Therefore, CEMNPs have huge potentialapplications in many fields, such as s MRI contrast agent, bio-analysis, drug carrier, mediumhigh heat therapy, catalyst, magnetic record, magnetic separation and so on. The preparation,properties and applied basic research of carbon encapsulated metal nano-particles as a newkind of carbon based nanocomposite have become a research hotspot.
A lot of methods have been developed for preparing carbon encapsulated metalnanoparticles. Currently, main preparation methods include high energy growing approach(such as electric arc, ion beam, laser and explosion), chemical vapor deposition and carbontransition. These methods have the features with high energy assumption, complex technicsand expensive prices. Moreover, the production rate is low for CEMNPs, especially forCEMNPs with magnetic cores, which limits the application and research interests ofCEMNPs.
In this study, different types of carbon encapsulated metal nanoparticles, includingcarbon encapsulated cobalt nanoparticles (assigned as Co@C), carbon encapsulated coppernickel nanoparticles (assigned as CuNi@C), were prepared using pyrolysis the precursorunder N2atmosphere which obtained by evaporating the mixture solution of sucrose andmetal nitrate to dryness, and the preparation scale was dozens of grams at a time. A newpreparation method for synthesis of the monodispersed CEMNPs samples, which was namedas liquid reduction-high temperature carbonization method, has been put forward bycombination of soft chemistry method and pyrolysis method.Some CEMNPs samples,including carbon encapsulated copper nickel nanoparticles (assigned as Cu@C), carbonencapsulated iron nanoparticles (assigned as Fe@C), carbon encapsulated cobaltnanoparticles [assigned as Co@C(LR)] and carbon encapsulated iron-copper nanoparticles(assigned as FeCu4@C), have been prepared by the developed method. The preparation amontis dozens of grams once. The chemical composition, phase, micro-structure and some majorphysical, chemical properties of as prepared CEMNPs samples were systematicallycharacterized by various modern analysis methods. The friction and wear properties of somekinds of the as-prepared CEMNPs samples were then studied by adding them into the atoleine as an additive of lubricating oil. The electrochemical catalytic performance was measuredthrough modifying a glassy carbon electrode in the electrochemical reaction of p-Nitrophenol.The following research results are obtained in this study.
The core of Co@C is fcc-Co while the shells are homocentrically hexagonal multi-layercarbon nets which are connected with some group, such as=O,-OH and so on. The dispersionparticle size is much bigger than that of observation under the transmission electronmicroscope (TEM) because there are some amorphous carbons being around of the Co@Cnanoparticles. Tthe average value of the former is equal to162.8nm and that of the latter isequal to35.3nm. The saturation magnetization, M_s, is equal to24.7emu/g under ambienttemperature measured using a vibrating specimen magnetometer (VSM), and the residualmagnetization, Mr=3.71emu/g, the magnetic coercive force, Hc=275.2Oe. The results ofTG-DSC test revealed that the metallic core of Co@C had been obviously oxygenated until1000℃for the protection of carbon shells. The sample of Co@C is an electrical conductorwhich resistivity is equal to9.46·cm under ambient temperature and there is absorbingcapacity for the microwave with the frequency of8～18GHz, the maximum is equal to6.36dB at the frequency of14.7GHz.
The shells of Co@C(LR) are composed of amorphous carbons, and the cores arepolycrystal of fcc-Co. The nanoparticles are monodispersion with an average particle size of49.6nm. Only less than1/5of the carbons in the as-prepared sample are connected withanother carbon atom, and all of the else are connected with other groups. The cobalt atoms arein two states too. That is, the vast majority of the cobalt atoms are the metallic state, and theothers are oxidation state. The sample of Co@C(LR) showed a quasi-superparamagnetismunder room temperature, and M_s=130.7emu/g, Mr=13.0emu/g, Hc=56Oe. The special surfacearea (SSA) measured using BET method is equal to167.0m2/g. The friction and wear testresults of adding the sample into the atoleine as an additive of lubricating oil showed that theCo@C(LR) had better performance of friction-reduction and anti-wear. The bearing capacityof the test oil has significantly increased when the additive amount of Co@C(LR) is0.6wt%,and the friction coefficient (μ) and wear rate (W) decrease to minimum when the additiveamount is0.4wt%, which are lower than that of the matched oil. The Co@C(LR) haspresented good catalytic activity in the electrochemical reaction of p-Nitrophenol (PNP) bycomparing the CV curves measured using a glassy carbon electrode (GCE) modified by theCo@C(LR) with that of measured using a bare GCE.
The core of CuNi@C is composed of the polycrystal of fcc-CuNi alloy and the shells are carbon of which the lattice fringes can be observed but no longer continuous and perfect. Thedispersion particle size is much bigger than that of observation under TEM because there aresome amorphous carbons being around of the CuNi@C nanoparticles. The average value ofthe former is equal to134.1nm and that of the latter is equal to55.0nm. The quantity ofcarbon atoms connected with another carbon atom is about one third and the else areconnected with other groups. All of the cobalt and nickel are in two states: metallic state andoxidation state. The CuNi@C is apoor electrical conductor whose resistivity is equal to100.56·cm under ambient temperature and there is absorbing capacity for the microwavewith the frequency of8～18GHz, the maximum is equal to8.1dB at the frequency of14.9GHz. The friction and wear test results of adding the sample into the atoleine as anadditive of lubricating oil showed that the CuNi@C had better performance offriction-reduction and antiwear. The friction coefficient and wear rate decrease to minimumwhen the additive amount of CuNi@C is0.6wt%, which are much lower than that of thematched oil.
The core of Fe@C is mainly composed of the polycrystal of bcc-Fe and the shells areamorphous carbons. The nanoparticles are monodispersion with an average particle size of48nm. The quantity of carbon atoms of the samples which are connected with another carbonatom is about43%and the others are connected with–OH=N and so on. The ratio of iron formetallic state is about76%, the valence state of other iron is Fe3+. The magnetic properties ofthe Fe@C measured by VSM are: M_s=54.56emu/g, Mr=5.35emu/g, Hc=205Oe. The specialsurface area measured by BET method is equal to522.7m2/g. The Fe@C has present goodcatalytic activity in the electrochemical reaction of p-Nitrophenol (PNP) and the bestconcentration of NaOH solution is1mol/L.
The core of Cu@C is mainly composed of the polycrystal of fcc-Cu and the shells areamorphous carbons, but the lattice fringe can be observed on local area. The nanoparticles aremonodispersion with an average particle size of49.5nm. The quantity of carbon atoms of thesamples which are connected with another carbon atom is about1/2and the else areconnected with other groups. The atoms of copper are in two states: metal and CuO. Thespecial surface area measured by BET method is equal to94.1m2/g. The friction and wear testresults of adding the sample into the atoleine as an additive of lubricating oil showed that theCu@C had better performance of friction-reduction and anti-wear. Compared with thematched oil, the friction coefficient decreased21.6%, the wear rate reduced30.0%when theadding amount was0.6wt%. The Cu@C has present good catalytic activity in theelectrochemical reaction of p-Nitrophenol (PNP) and the best concentration of NaOH solution is0.5mol/L.
The core of FeCu4@C is mainly composed of the polycrystal of fcc-FeCu4and the shellsare amorphous carbons. The nanoparticles are monodispersion with an average particle size of62.8nm. The ratio of carbon atoms of the samples which are connected with another carbonatom is about36%and the else are connected with other groups. The atoms of copper are intwo states: metal and Cu(OH)2. The content of iron is very lower so only the metallic state hasbeen detected. The magnetic properties of the Fe Cu4@C measured by VSM are:M_s=13.01emu/g, Mr=0.37emu/g, Hc=54.43Oe. The special surface area measured by BETmethod is equal to269.9m2/g.
The knowledge for the preparation, characterization and tribology of carbonencapsulated metal nanoparticles gained in this study would enrichthe basic theory ofCEMNPs and promote the application of CEMNPs.
本文以价格低廉、获取方便的蔗糖和金属硝酸盐为主要原料，首先采用热解法在N2气氛下制备出碳包覆钴纳米粒子(记为Co@C)、碳包覆铜镍纳米粒子(记为CuNi@C)；在此基础上，将软化学方法和热解法与结合，提出了液相还原-高温炭化法，制备出碳包覆铜纳米粒子(记为Cu@C)、碳包覆铁纳米粒子(记为Fe@C)、碳包覆钴纳米粒子[记为Co@C(LR)]和碳包覆铁铜纳米粒子(记为FeCu_4@C)，实现了CEMNPs成单分散状。对所制备的CEMNPs，采用多种现代分析测试方法对其化学组成、物相、显微结构和一些主要物理、化学性质进行了较为系统的表征，试验研究了碳包覆金属纳米粒子作为润滑油添加剂对摩擦磨损性能的影响；探讨了碳包覆金属纳米粒子修饰玻碳电极的电化学催化性能。研究结果表明：
Co@C的核为fcc-Co、壳为多层同心层状六角形碳网，在碳网上连接有=O、-OH等基团。在Co@C纳米粒子外围存在无定形碳，分散粒径均值162.8nm， TEM测定粒径均值35.3nm。室温下其饱和磁化强度M_s=24.7emu/g，剩余磁化强度M_r=3.71emu/g，矫顽力H_c=275.2Oe。碳壳保护作用明显，金属核在1000℃后才氧化。Co@C具有一定的导电性，常温电阻率9.46·cm。对于8～18GHz微波具有一定的吸收能力，在14.7GHz时吸收最大为6.36dB。
Co@C(LR)壳层为无定形碳，核为多晶fcc-Co，基本呈单分散状，平均粒径49.6nm。样品中不足1/5的碳为纯C-C结合，其余均连接有其它基团，钴核主要呈现0价金属态和少量氧化态。室温下Co@C(LR)的M_s=130.7emu/g、M_r=13.0emu/g，H_c=56Oe，表现出超顺磁性。BET法测试的Co@C(LR)比表面积SSA=167.0m2/g。在液体石蜡中添加Co@C进行的摩擦磨损试验发现：当添加量为0.6wt%时其承载力有所提高，添加量为0.4wt%时摩擦系数μ和磨痕宽度W最小，均低于对照油，说明Co@C(LR)有一定的减摩抗磨效果。对比以裸玻碳电极(GCE)和以Co@C(LR)修饰的GCE为工作电极时得到的CV曲线，Co@C(LR)对对硝基苯酚(PNP)的电化学反应有良好的催化效果。
CuNi@C的核为多晶fcc-CuNi合金，壳为可观察到石墨结构层的C，但晶格条纹不够连续、完整。壳外粘连有无定形碳，其分散粒径为134.1nm、TEM测试粒径为55nm。样品中约1/3的碳为纯C-C结合，余下的都与其它基团有相互作用，Cu、Ni都存在金属态和氧化态两种形式。CuNi@C有一定的导电性，室温电阻率为100.56Ω cm，对于8～18GHz微波具有一定的吸收能力，在14.9GHz时吸收最大为8.1dB。将CuNi@C添加到液体石蜡中进行的摩擦磨损试验结果表明，当添加量为0.6wt%时有效降低了摩擦系数μ和磨痕宽度W，表现出了较好的减摩抗磨性能。
Fe@C的核主要是多晶bcc-Fe，壳为无定形碳，为单分散状，平均粒径48nm。样品中约43%的碳为C-C结合，其余与其-OH、-N有相互作用，约76%的Fe为0价金属，其余为Fe~(3+)。磁性能测试结果为：M_s=54.56emu/g，M_r=5.35emu/g， H_c=205Oe。BET法测得的SSA=522.7m~2/g。Fe@C对PNP的电化学反应有良好的催化效果，最佳NaOH浓度为1mol/L。
Cu@C的核为多晶fcc-Cu，壳为无定形碳，局部能观察到晶格条纹，单分散状，平均粒径49.5nm。约1/2的C为纯C-C连接，其余的连接有其它基团，Cu有0价金属和CuO两种状态。BET法测得的SSA=94.1m~2/g。在液体石蜡中添加一定量的Cu@C具有明显的减摩抗磨效果，当添加量为0.6wt%时，与对照油相比μ降低了21.6%，W降低了30.0%。Cu@C对PNP的电化学反应有良好的催化效果，最佳NaOH浓度为0.5mol/L。
FeCu_4@C的核为fcc-FeCu_4，壳为无定形碳，单分散状，平均粒径62.8nm。约36%的C为纯C-C连接，其余的连接有其它基团，Cu有0价金属和Cu(OH)_2两种状态，Fe含量低，只检测到0价金属态。磁性能测试结果为：M_s=13.01emu/g，M_r=0.37emu/g，H_c=54.43Oe。BET法测得的SSA=269.9m~2/g。
基于上述研究工作在碳包覆金属纳米粒子制备方法、性能表征和摩擦学性能研究等方面获得的知识，丰富了碳包覆金属纳米材料的基础理论，在促进应用技术发展方面提供了支持。
Carbon encapsulated metal nano-particles (CEMNPs)are types of carbon/metalcomposite materials with core/shell structure in nanoscale. The different combination ofvarious metal nanometer materials as core and carbon as shell rewards the composite withmany peculiar physical and chemical properties.Therefore, CEMNPs have huge potentialapplications in many fields, such as s MRI contrast agent, bio-analysis, drug carrier, mediumhigh heat therapy, catalyst, magnetic record, magnetic separation and so on. The preparation,properties and applied basic research of carbon encapsulated metal nano-particles as a newkind of carbon based nanocomposite have become a research hotspot.
A lot of methods have been developed for preparing carbon encapsulated metalnanoparticles. Currently, main preparation methods include high energy growing approach(such as electric arc, ion beam, laser and explosion), chemical vapor deposition and carbontransition. These methods have the features with high energy assumption, complex technicsand expensive prices. Moreover, the production rate is low for CEMNPs, especially forCEMNPs with magnetic cores, which limits the application and research interests ofCEMNPs.
In this study, different types of carbon encapsulated metal nanoparticles, includingcarbon encapsulated cobalt nanoparticles (assigned as Co@C), carbon encapsulated coppernickel nanoparticles (assigned as CuNi@C), were prepared using pyrolysis the precursorunder N2atmosphere which obtained by evaporating the mixture solution of sucrose andmetal nitrate to dryness, and the preparation scale was dozens of grams at a time. A newpreparation method for synthesis of the monodispersed CEMNPs samples, which was namedas liquid reduction-high temperature carbonization method, has been put forward bycombination of soft chemistry method and pyrolysis method.Some CEMNPs samples,including carbon encapsulated copper nickel nanoparticles (assigned as Cu@C), carbonencapsulated iron nanoparticles (assigned as Fe@C), carbon encapsulated cobaltnanoparticles [assigned as Co@C(LR)] and carbon encapsulated iron-copper nanoparticles(assigned as FeCu4@C), have been prepared by the developed method. The preparation amontis dozens of grams once. The chemical composition, phase, micro-structure and some majorphysical, chemical properties of as prepared CEMNPs samples were systematicallycharacterized by various modern analysis methods. The friction and wear properties of somekinds of the as-prepared CEMNPs samples were then studied by adding them into the atoleine as an additive of lubricating oil. The electrochemical catalytic performance was measuredthrough modifying a glassy carbon electrode in the electrochemical reaction of p-Nitrophenol.The following research results are obtained in this study.
The core of Co@C is fcc-Co while the shells are homocentrically hexagonal multi-layercarbon nets which are connected with some group, such as=O,-OH and so on. The dispersionparticle size is much bigger than that of observation under the transmission electronmicroscope (TEM) because there are some amorphous carbons being around of the Co@Cnanoparticles. Tthe average value of the former is equal to162.8nm and that of the latter isequal to35.3nm. The saturation magnetization, M_s, is equal to24.7emu/g under ambienttemperature measured using a vibrating specimen magnetometer (VSM), and the residualmagnetization, Mr=3.71emu/g, the magnetic coercive force, Hc=275.2Oe. The results ofTG-DSC test revealed that the metallic core of Co@C had been obviously oxygenated until1000℃for the protection of carbon shells. The sample of Co@C is an electrical conductorwhich resistivity is equal to9.46·cm under ambient temperature and there is absorbingcapacity for the microwave with the frequency of8～18GHz, the maximum is equal to6.36dB at the frequency of14.7GHz.
The shells of Co@C(LR) are composed of amorphous carbons, and the cores arepolycrystal of fcc-Co. The nanoparticles are monodispersion with an average particle size of49.6nm. Only less than1/5of the carbons in the as-prepared sample are connected withanother carbon atom, and all of the else are connected with other groups. The cobalt atoms arein two states too. That is, the vast majority of the cobalt atoms are the metallic state, and theothers are oxidation state. The sample of Co@C(LR) showed a quasi-superparamagnetismunder room temperature, and M_s=130.7emu/g, Mr=13.0emu/g, Hc=56Oe. The special surfacearea (SSA) measured using BET method is equal to167.0m2/g. The friction and wear testresults of adding the sample into the atoleine as an additive of lubricating oil showed that theCo@C(LR) had better performance of friction-reduction and anti-wear. The bearing capacityof the test oil has significantly increased when the additive amount of Co@C(LR) is0.6wt%,and the friction coefficient (μ) and wear rate (W) decrease to minimum when the additiveamount is0.4wt%, which are lower than that of the matched oil. The Co@C(LR) haspresented good catalytic activity in the electrochemical reaction of p-Nitrophenol (PNP) bycomparing the CV curves measured using a glassy carbon electrode (GCE) modified by theCo@C(LR) with that of measured using a bare GCE.
The core of CuNi@C is composed of the polycrystal of fcc-CuNi alloy and the shells are carbon of which the lattice fringes can be observed but no longer continuous and perfect. Thedispersion particle size is much bigger than that of observation under TEM because there aresome amorphous carbons being around of the CuNi@C nanoparticles. The average value ofthe former is equal to134.1nm and that of the latter is equal to55.0nm. The quantity ofcarbon atoms connected with another carbon atom is about one third and the else areconnected with other groups. All of the cobalt and nickel are in two states: metallic state andoxidation state. The CuNi@C is apoor electrical conductor whose resistivity is equal to100.56·cm under ambient temperature and there is absorbing capacity for the microwavewith the frequency of8～18GHz, the maximum is equal to8.1dB at the frequency of14.9GHz. The friction and wear test results of adding the sample into the atoleine as anadditive of lubricating oil showed that the CuNi@C had better performance offriction-reduction and antiwear. The friction coefficient and wear rate decrease to minimumwhen the additive amount of CuNi@C is0.6wt%, which are much lower than that of thematched oil.
The core of Fe@C is mainly composed of the polycrystal of bcc-Fe and the shells areamorphous carbons. The nanoparticles are monodispersion with an average particle size of48nm. The quantity of carbon atoms of the samples which are connected with another carbonatom is about43%and the others are connected with–OH=N and so on. The ratio of iron formetallic state is about76%, the valence state of other iron is Fe3+. The magnetic properties ofthe Fe@C measured by VSM are: M_s=54.56emu/g, Mr=5.35emu/g, Hc=205Oe. The specialsurface area measured by BET method is equal to522.7m2/g. The Fe@C has present goodcatalytic activity in the electrochemical reaction of p-Nitrophenol (PNP) and the bestconcentration of NaOH solution is1mol/L.
The core of Cu@C is mainly composed of the polycrystal of fcc-Cu and the shells areamorphous carbons, but the lattice fringe can be observed on local area. The nanoparticles aremonodispersion with an average particle size of49.5nm. The quantity of carbon atoms of thesamples which are connected with another carbon atom is about1/2and the else areconnected with other groups. The atoms of copper are in two states: metal and CuO. Thespecial surface area measured by BET method is equal to94.1m2/g. The friction and wear testresults of adding the sample into the atoleine as an additive of lubricating oil showed that theCu@C had better performance of friction-reduction and anti-wear. Compared with thematched oil, the friction coefficient decreased21.6%, the wear rate reduced30.0%when theadding amount was0.6wt%. The Cu@C has present good catalytic activity in theelectrochemical reaction of p-Nitrophenol (PNP) and the best concentration of NaOH solution is0.5mol/L.
The core of FeCu4@C is mainly composed of the polycrystal of fcc-FeCu4and the shellsare amorphous carbons. The nanoparticles are monodispersion with an average particle size of62.8nm. The ratio of carbon atoms of the samples which are connected with another carbonatom is about36%and the else are connected with other groups. The atoms of copper are intwo states: metal and Cu(OH)2. The content of iron is very lower so only the metallic state hasbeen detected. The magnetic properties of the Fe Cu4@C measured by VSM are:M_s=13.01emu/g, Mr=0.37emu/g, Hc=54.43Oe. The special surface area measured by BETmethod is equal to269.9m2/g.
The knowledge for the preparation, characterization and tribology of carbonencapsulated metal nanoparticles gained in this study would enrichthe basic theory ofCEMNPs and promote the application of CEMNPs.
引文
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