基于无机氧化物的核壳型功能纳米复合材料的合成及其性能研究
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摘要
癌症是严重威胁人类健康的疾病,据联合国世界卫生组织(WHO)统计,由于生活环境,饮食习惯等诸多因素,癌症发病率逐年增高,目前我国每年因肿瘤而死亡的人数达150万。而癌症的治疗却一直是医学界难以攻克的难题,为此,诸如阿霉素,紫杉醇等一系列具有良好药效的化疗药物被相继开发并应用于肿瘤的临床治疗中。但由于这些药物大多缺乏专一药理作用,不能对肿瘤细胞或组织有的放矢,在实际临床应用中存在着严重的毒副作用。这不仅给患者带来了极大的痛苦,也降低了药物的生物利用率。因此,如何实现药物的高效安全负载及可控释放已成为当今生物医学领域研究的重点前沿和焦点之一。
本论文主要针对目前抗肿瘤药物载体载药量小、功能单一等问题设计并制备了一系列基于功能聚合物的智能型药物控释体系。该类载体的优势在于其本身具有良好的生物相容性并在生物体内稳定循环,在达到指定的肿瘤部位后在特定的外部刺激条件下释放所负载的药物。与此同时,四氧化三铁(Fe304)纳米粒子的顺磁性或者表面修饰的聚合物的荧光性能还赋予该类纳米载体以磁共振造影或者荧光细胞成像功能,从而达到对肿瘤诊断及靶向治疗的双重目的。
(1)设计合成了以Fe304纳米粒子为核、靶向性荧光聚合物(PMA-RBM-FA)为壳的纳米复合物(Fe3O4@mSiO2@PMA-RBM-FA)。首先合成了粒径分布均一的Fe304纳米粒子,并在其表面包裹一层介孔二氧化硅(mSiO2)以增加其生物相容性。另外合成了一种新型水溶性荧光聚合物PMA-RBM,通过KH550接枝到Fe3O4@mSiO2表面,利用mSiO2的孔道吸附性能以及亲水性荧光聚合物(PMA-RBM)的氢键负载药物,然后通过活性酯与氨基反应在复合纳米粒子表面修饰上叶酸(Folic Acid),对叶酸高表达的肿瘤细胞实现靶向药物输送。另外,Fe3O4@mSiO2@PMA-RBM-FA通过透过性增强及滞留(EPR)效应在肿瘤组织部位富集的同时,可以方便地利用磁共振成像(MRI)以及荧光成像来作为体内以及体外诊断的工具,从而简便地实现肿瘤的诊断与治疗的双重目的。该核-壳型纳米复合物将无机纳米材料与功能性聚合物的优点相结合,改善了聚合物药物载体在体内高盐环境中循环时的不稳定性以及现有纳米材料功能比较单一的缺陷,为聚合物-无机纳米复合药物载体的进一步发展作了良好的铺垫。
(2)为了更好地实现药物的pH响应智能型控制释放及磁共振造影诊断,我们在核-壳型纳米复合物的聚合物壳层引入基于缩醛结构的pH-敏感基团。首先设计合成具有良好生物相容性的pH-敏感两亲性聚合物,并在水介质中与油酸包裹的Fe304磁性纳米粒子(SPIONPs)通过疏水范德华力进行自组装,得到以Fe304核、pH-敏感两亲聚合物为壳的纳米复合物SPIONPs@PDH。该类药物载体具有良好的水相分散性,在组装过程中包裹疏水性药物并携带药物进入肿瘤部位,在肿瘤内部偏酸性环境刺激下即发生降解,疏水的Fe304磁性纳米粒子也逐渐聚集而导致MRI信号发生明显的变化,最终实现肿瘤组织的选择性MRI诊断与治疗。
(3)利用可逆加成-断裂链转移(RAFT)的活性可控聚合方法控制聚合物分子量及分布指数,合成含有叶酸靶向基团的pH-敏感两亲性聚合物,并与Fe304磁性纳米粒子自组装,得到结构更可控、粒径更均一的pH-敏感肿瘤靶向核-壳型纳米复合物(HAMAFA-b-DBAM-SPIONPs)。组装过程中负载的药物可由该载体靶向输送到肿瘤部位并在肿瘤内部偏酸性环境刺激下释放。在保证上一体系的良好造影诊断及药物控释性能的基础上,该纳米药物载体更有利于实现对其结构的控制和药物的靶向输送。
(4)为了进一步突破纳米药物载体的载药效率,我们设计制备了具有中空介孔结构的二氧化硅(HMS)纳米粒子,其中空内腔以及介孔孔道可以极大地负载药物,从而有效提高载药量。另外,二氧化硅材料本身良好的生物相容性及表面可修饰性使其在纳米药物载体方面有更加广泛的应用前景。首先制备了疏水性荧光中空介孔二氧化硅(FOFHMS)纳米粒子,并利用范德华力将疏水性药物分子负载在其纳米内腔及孔道中,后包覆上两亲性的pH敏感靶向包裹剂起到封存药物的效果。该纳米药物载体在体内循环过程中可以选择性地富集于肿瘤细胞内并在肿瘤内部偏酸性条件刺激下实现药物的可控释放。体系中荧光素的引入赋予该纳米载体荧光造影功能,从而在输送药物的同时实现对肿瘤细胞的荧光监测与诊断。
上述基于四氧化三铁和二氧化硅无机纳米粒子的纳米复合材料除了在生物医用领域有良好的应用前景之外,由于其在电容量方面的优势,经改造后也可用于锂离子电池阳极材料的制备。在锂离子电池阳极纳米复合材料制备方面开展了研究,并取得了如下成果：
(5)将柔韧性优异的中空多孔四氧化三铁纳米粒子(HM)包覆上导电性优良、柔韧性很好的石墨烯材料来弥补其充放电过程中结构不稳定性的缺陷。此外,HM具有价格便宜、自然界大量存在等天然优势,相比目前使用的石墨电极(372mAhg-1)具有很高的比电容。实验结果表明,通过简易的静电组装得到的锂离子阳极材料具有优异的电容(大于900mAh g-1)并保持良好的充放电循环性能(循环90次后仍保持在832mAhg-1)。
(6)为了进一步提高电极材料的电容,进而提高锂离子电池的电池容量(从900mAh g-1增加到3762mAhg-1),我们将中空多孔二氧化硅通过简便的镁热还原法得到中空多孔的硅材料,然后通过简单的银镜反应将银纳米粒子修饰到中空多孔硅材料孔道及内腔,以提高硅纳米粒子间的电子导通能力。该方法通过简单的途径得到高性能的硅基阳极材料,为降低硅基阳极材料成本、提高锂离子电池容量以及实现高容量锂离子电池的工业化等提供了切实有效的途径。
Cancer is a serious threat to human health and disease. According to the statistics of the United Nations World Health Organization (WHO), the incidence of cancer increased year by year because of the living environments, eating habits and so on. And in China, the annual number of deaths was around1.5million. However, the treatment of cancer was still difficult to overcome in medicine. Then, a series of chemotherapy drugs (doxorubicine, taxol, et al) with good efficacy were exploited and used in clinic. However, these drugs are mostly lack of specific pharmacological effects and exist serious side effects. This makes the patients treated with more physical burden, and drug bioavailability is very low. Thus, how to achieve efficient loading and controlled release of drugs has become a serious issue placed in front of the scientists and has become today's focus in the biomedical research field. In this thesis, we fabricated a series of intelligent drug delivery system to resolve the problems such as low drug loading capacity, functionality limitations, and so on. Our approach has excellent biocompatibility and stability and could accumulate in tumor sites. Then, the drug carriers would trigger release the loaded drugs and finally cure the cancer.
(1) Biocompatible and water-soluble magnetic nanoparticles with core (Fe3O4)-mesoporous shell (mSiO2) structure were prepared and successfully modified with the flourescent polymer chain as labeling segments and folic acid as cancer targeting moieties and loaded drug for directional release. The porous silica oxide structure and long molecular chains of polymethacrylic acid embedded drug efficiently in the nanocomposites and did not affect the magnetic properties of the carrier. Sustained release of the loaded drug was observed under in vitro conditions. Furthermore, the drug carrier is able to drill into the cell membranes and obtain a sustained release of anti-cancer drug in cytoplasm. The in vitro cellular uptake of drug demonstrated that the drug-loaded nanocomposites could effectively target to the tumor cells to cure it. Our model experiments indicated that the multifunctional mesoporous core-shell magnetic nanoparticle can be exploited as an anti-cancer drug delivery vehicle for targeting and therapy applications.
(2) A water-soluble, pH-responsive copolymer was synthesized successfully and used as a polymeric-carrier to deliver hydrophobic paramagnetic nanoparticles into cells. In an acidic environment, the nanoparticles aggregate as the copolymer degrades, resulting in the enhancement of an in vitro MRI signal. A novel long-chain monomer was synthesized and then polymerized with a water-soluble monomer. The as-synthesized amphiphilic copolymer drug carrier has excellent biocompatibility and degradability properties. The hydrophobic copolymer side-chain can insert into the oleic acid with the hydrophilic part on the surface to form water-soluble nanocomposites. Furthermore, this composite can also easily load hydrophobic drugs via hydrophobic interactions. Degradation of the polymer shell under weakly acidic conditions leads to the release of the SPIONPs and drugs from the polymeric carrier, resulting in the MRI signal switching and drug release, respectively. Our approach can achieve these outstanding dual functions, tumor diagnosis and therapy.
(3) Multifunctional drug delivery systems with favorable compatibility, high selectivity and efficiency are appropriate candidates for future medical applications. For this purpose, a multifunctional nanocomposite that enables selective magnetic resonance imaging and anticancer therapy by encapsulating hydrophobic superparamagnetic nanoparticles and chemotherapeutic agent doxorubicin with a novel biodegradable pH-activated polymeric carrier was synthesized. The as-synthesized amphiphilic polymer has excellent biocompatibility and pH-responsibility. The obtained nanocomposites selectively release the encapsulated drug and magnetic nanoparticles in mild acidic endosomal/lysosomal compartments due to the degradation of the pH-responsive bonds, resulting in a change of imaging signal and cancer therapy. Furthermore, when compared with the nanocomposites without targeting moiety, as studied from over-express the folic acid receptor tumor cell culturing, the conjugates with folic acid showed a significantly more potent targeting capability.
(4) We fabricated a novel multifunctional nanocomposites consisting of hydrophobic HMSNPs and folate-conjugated amphiphilic capping agent for receptor-mediated controlled drug release. The first step was the synthesis of HMSNPs using polystyrene (PS) as template and tetraethyl orthosilicate (TEOS) as the Si source. Then the surface of HMSNPs was coated with a widely used fluorescent probe for optical imaging. The obtained fluorescent HMSNPs were modified with the long-chain hydrophobic moieties octadecyltrimethoxysilane (C18), which could change the wettability of the surface (from highly hydrophilic to hydrophobic), increase the amount of hydrophobic drug adsorption and further delay the drug release. The second step was the self-assembly of hydrophobic HMSNPs, drugs and folate-conjugated amphiphilic capping agent, which could effectively decrease clearance by reticuloendothelial system (RES), prevent drug carriers'aggregation, and interface with cellular uptake by steric hindrance. After the hydrophobic and van der Waals interactions between the alkyl chains (C18from hydrophobic HMSNPs and C12from amphiphilic capping agent), the hydrophobic drug could be loaded in HMSNPs and blocked by capping agent. The obtained multifunctional nanocomposites could be well dispersed in aqueous solution. When specifically recognized and internalized by folate receptor (FR) over-expressed tumor cells, the pH-responsive shell would hydrolyzed due to cleavage of acetal moieties in the weakly acidic endosomal/lysosomal compartments, resulting in loaded drug release. Thus, our approach can achieve these outstanding functions, tumor targeting, diagnosis and therapy.
Based on the above works, we further studied the potential applications of hollow porous iron oxide and silica in lithium-ion anode materials.
(5) Graphene-encapsulated ordered aggregates of Fe3O4nanoparticles with nearly-spherical geometry and hollow interior were synthesized by a simple self-assembly process. We combine the unique properties of graphene sheets and a hollow assembly of nanoparticles to simultaneously provide a large reversible Li+storage capacity, good rate performance and long cycle life. A simple self-assembly process driven by electrostatic interaction was used to generate graphene-encapsulated hollow Fe3O4nanoparticle aggregates (G-HM, short for graphene-encapsulated hollow magnetite particles). In this process, graphene oxide and HM nanoparticle aggregates were first modified to acquire negative and positive charged respectively. The assembly was carried out under very mild reaction conditions and consequently perturbations to the intrinsic properties of the HM nanoparticles could be kept to a minimum. The G-HM composite particles synthesized as such showed remarkable cycle stability as well as lithium storage performance compared to the pristine HM nanoparticles or a mixture of graphene and HM particles. The graphene modification of porous nanoparticle aggregates is therefore a viable and facile approach to prepare high performance anode materials for the lithium ion batteries.
(6) We report a facile approach to fabricate monodisperse hollow porous Si (HPSi) nanoparticles (～120nm) via the magnesiothermic reduction of hollow porous SiO2(HPSiO2) nanoparticles formed by a templating method. This is followed by Ag nanoparticle coating for conductivity enhancement. The HPSi anode prepared as such shows several desirable electrochemical features:a high specific reversible capacity (3762mAh g-1), good cycle stability (>93%capacity retention after99cycles), and good rate performance (>2000mAh g-1at4000mA g-1), surpassing the performance of anode materials based on micron size macroporous Si particles.
本论文主要针对目前抗肿瘤药物载体载药量小、功能单一等问题设计并制备了一系列基于功能聚合物的智能型药物控释体系。该类载体的优势在于其本身具有良好的生物相容性并在生物体内稳定循环,在达到指定的肿瘤部位后在特定的外部刺激条件下释放所负载的药物。与此同时,四氧化三铁(Fe304)纳米粒子的顺磁性或者表面修饰的聚合物的荧光性能还赋予该类纳米载体以磁共振造影或者荧光细胞成像功能,从而达到对肿瘤诊断及靶向治疗的双重目的。
(1)设计合成了以Fe304纳米粒子为核、靶向性荧光聚合物(PMA-RBM-FA)为壳的纳米复合物(Fe3O4@mSiO2@PMA-RBM-FA)。首先合成了粒径分布均一的Fe304纳米粒子,并在其表面包裹一层介孔二氧化硅(mSiO2)以增加其生物相容性。另外合成了一种新型水溶性荧光聚合物PMA-RBM,通过KH550接枝到Fe3O4@mSiO2表面,利用mSiO2的孔道吸附性能以及亲水性荧光聚合物(PMA-RBM)的氢键负载药物,然后通过活性酯与氨基反应在复合纳米粒子表面修饰上叶酸(Folic Acid),对叶酸高表达的肿瘤细胞实现靶向药物输送。另外,Fe3O4@mSiO2@PMA-RBM-FA通过透过性增强及滞留(EPR)效应在肿瘤组织部位富集的同时,可以方便地利用磁共振成像(MRI)以及荧光成像来作为体内以及体外诊断的工具,从而简便地实现肿瘤的诊断与治疗的双重目的。该核-壳型纳米复合物将无机纳米材料与功能性聚合物的优点相结合,改善了聚合物药物载体在体内高盐环境中循环时的不稳定性以及现有纳米材料功能比较单一的缺陷,为聚合物-无机纳米复合药物载体的进一步发展作了良好的铺垫。
(2)为了更好地实现药物的pH响应智能型控制释放及磁共振造影诊断,我们在核-壳型纳米复合物的聚合物壳层引入基于缩醛结构的pH-敏感基团。首先设计合成具有良好生物相容性的pH-敏感两亲性聚合物,并在水介质中与油酸包裹的Fe304磁性纳米粒子(SPIONPs)通过疏水范德华力进行自组装,得到以Fe304核、pH-敏感两亲聚合物为壳的纳米复合物SPIONPs@PDH。该类药物载体具有良好的水相分散性,在组装过程中包裹疏水性药物并携带药物进入肿瘤部位,在肿瘤内部偏酸性环境刺激下即发生降解,疏水的Fe304磁性纳米粒子也逐渐聚集而导致MRI信号发生明显的变化,最终实现肿瘤组织的选择性MRI诊断与治疗。
(3)利用可逆加成-断裂链转移(RAFT)的活性可控聚合方法控制聚合物分子量及分布指数,合成含有叶酸靶向基团的pH-敏感两亲性聚合物,并与Fe304磁性纳米粒子自组装,得到结构更可控、粒径更均一的pH-敏感肿瘤靶向核-壳型纳米复合物(HAMAFA-b-DBAM-SPIONPs)。组装过程中负载的药物可由该载体靶向输送到肿瘤部位并在肿瘤内部偏酸性环境刺激下释放。在保证上一体系的良好造影诊断及药物控释性能的基础上,该纳米药物载体更有利于实现对其结构的控制和药物的靶向输送。
(4)为了进一步突破纳米药物载体的载药效率,我们设计制备了具有中空介孔结构的二氧化硅(HMS)纳米粒子,其中空内腔以及介孔孔道可以极大地负载药物,从而有效提高载药量。另外,二氧化硅材料本身良好的生物相容性及表面可修饰性使其在纳米药物载体方面有更加广泛的应用前景。首先制备了疏水性荧光中空介孔二氧化硅(FOFHMS)纳米粒子,并利用范德华力将疏水性药物分子负载在其纳米内腔及孔道中,后包覆上两亲性的pH敏感靶向包裹剂起到封存药物的效果。该纳米药物载体在体内循环过程中可以选择性地富集于肿瘤细胞内并在肿瘤内部偏酸性条件刺激下实现药物的可控释放。体系中荧光素的引入赋予该纳米载体荧光造影功能,从而在输送药物的同时实现对肿瘤细胞的荧光监测与诊断。
上述基于四氧化三铁和二氧化硅无机纳米粒子的纳米复合材料除了在生物医用领域有良好的应用前景之外,由于其在电容量方面的优势,经改造后也可用于锂离子电池阳极材料的制备。在锂离子电池阳极纳米复合材料制备方面开展了研究,并取得了如下成果：
(5)将柔韧性优异的中空多孔四氧化三铁纳米粒子(HM)包覆上导电性优良、柔韧性很好的石墨烯材料来弥补其充放电过程中结构不稳定性的缺陷。此外,HM具有价格便宜、自然界大量存在等天然优势,相比目前使用的石墨电极(372mAhg-1)具有很高的比电容。实验结果表明,通过简易的静电组装得到的锂离子阳极材料具有优异的电容(大于900mAh g-1)并保持良好的充放电循环性能(循环90次后仍保持在832mAhg-1)。
(6)为了进一步提高电极材料的电容,进而提高锂离子电池的电池容量(从900mAh g-1增加到3762mAhg-1),我们将中空多孔二氧化硅通过简便的镁热还原法得到中空多孔的硅材料,然后通过简单的银镜反应将银纳米粒子修饰到中空多孔硅材料孔道及内腔,以提高硅纳米粒子间的电子导通能力。该方法通过简单的途径得到高性能的硅基阳极材料,为降低硅基阳极材料成本、提高锂离子电池容量以及实现高容量锂离子电池的工业化等提供了切实有效的途径。
Cancer is a serious threat to human health and disease. According to the statistics of the United Nations World Health Organization (WHO), the incidence of cancer increased year by year because of the living environments, eating habits and so on. And in China, the annual number of deaths was around1.5million. However, the treatment of cancer was still difficult to overcome in medicine. Then, a series of chemotherapy drugs (doxorubicine, taxol, et al) with good efficacy were exploited and used in clinic. However, these drugs are mostly lack of specific pharmacological effects and exist serious side effects. This makes the patients treated with more physical burden, and drug bioavailability is very low. Thus, how to achieve efficient loading and controlled release of drugs has become a serious issue placed in front of the scientists and has become today's focus in the biomedical research field. In this thesis, we fabricated a series of intelligent drug delivery system to resolve the problems such as low drug loading capacity, functionality limitations, and so on. Our approach has excellent biocompatibility and stability and could accumulate in tumor sites. Then, the drug carriers would trigger release the loaded drugs and finally cure the cancer.
(1) Biocompatible and water-soluble magnetic nanoparticles with core (Fe3O4)-mesoporous shell (mSiO2) structure were prepared and successfully modified with the flourescent polymer chain as labeling segments and folic acid as cancer targeting moieties and loaded drug for directional release. The porous silica oxide structure and long molecular chains of polymethacrylic acid embedded drug efficiently in the nanocomposites and did not affect the magnetic properties of the carrier. Sustained release of the loaded drug was observed under in vitro conditions. Furthermore, the drug carrier is able to drill into the cell membranes and obtain a sustained release of anti-cancer drug in cytoplasm. The in vitro cellular uptake of drug demonstrated that the drug-loaded nanocomposites could effectively target to the tumor cells to cure it. Our model experiments indicated that the multifunctional mesoporous core-shell magnetic nanoparticle can be exploited as an anti-cancer drug delivery vehicle for targeting and therapy applications.
(2) A water-soluble, pH-responsive copolymer was synthesized successfully and used as a polymeric-carrier to deliver hydrophobic paramagnetic nanoparticles into cells. In an acidic environment, the nanoparticles aggregate as the copolymer degrades, resulting in the enhancement of an in vitro MRI signal. A novel long-chain monomer was synthesized and then polymerized with a water-soluble monomer. The as-synthesized amphiphilic copolymer drug carrier has excellent biocompatibility and degradability properties. The hydrophobic copolymer side-chain can insert into the oleic acid with the hydrophilic part on the surface to form water-soluble nanocomposites. Furthermore, this composite can also easily load hydrophobic drugs via hydrophobic interactions. Degradation of the polymer shell under weakly acidic conditions leads to the release of the SPIONPs and drugs from the polymeric carrier, resulting in the MRI signal switching and drug release, respectively. Our approach can achieve these outstanding dual functions, tumor diagnosis and therapy.
(3) Multifunctional drug delivery systems with favorable compatibility, high selectivity and efficiency are appropriate candidates for future medical applications. For this purpose, a multifunctional nanocomposite that enables selective magnetic resonance imaging and anticancer therapy by encapsulating hydrophobic superparamagnetic nanoparticles and chemotherapeutic agent doxorubicin with a novel biodegradable pH-activated polymeric carrier was synthesized. The as-synthesized amphiphilic polymer has excellent biocompatibility and pH-responsibility. The obtained nanocomposites selectively release the encapsulated drug and magnetic nanoparticles in mild acidic endosomal/lysosomal compartments due to the degradation of the pH-responsive bonds, resulting in a change of imaging signal and cancer therapy. Furthermore, when compared with the nanocomposites without targeting moiety, as studied from over-express the folic acid receptor tumor cell culturing, the conjugates with folic acid showed a significantly more potent targeting capability.
(4) We fabricated a novel multifunctional nanocomposites consisting of hydrophobic HMSNPs and folate-conjugated amphiphilic capping agent for receptor-mediated controlled drug release. The first step was the synthesis of HMSNPs using polystyrene (PS) as template and tetraethyl orthosilicate (TEOS) as the Si source. Then the surface of HMSNPs was coated with a widely used fluorescent probe for optical imaging. The obtained fluorescent HMSNPs were modified with the long-chain hydrophobic moieties octadecyltrimethoxysilane (C18), which could change the wettability of the surface (from highly hydrophilic to hydrophobic), increase the amount of hydrophobic drug adsorption and further delay the drug release. The second step was the self-assembly of hydrophobic HMSNPs, drugs and folate-conjugated amphiphilic capping agent, which could effectively decrease clearance by reticuloendothelial system (RES), prevent drug carriers'aggregation, and interface with cellular uptake by steric hindrance. After the hydrophobic and van der Waals interactions between the alkyl chains (C18from hydrophobic HMSNPs and C12from amphiphilic capping agent), the hydrophobic drug could be loaded in HMSNPs and blocked by capping agent. The obtained multifunctional nanocomposites could be well dispersed in aqueous solution. When specifically recognized and internalized by folate receptor (FR) over-expressed tumor cells, the pH-responsive shell would hydrolyzed due to cleavage of acetal moieties in the weakly acidic endosomal/lysosomal compartments, resulting in loaded drug release. Thus, our approach can achieve these outstanding functions, tumor targeting, diagnosis and therapy.
Based on the above works, we further studied the potential applications of hollow porous iron oxide and silica in lithium-ion anode materials.
(5) Graphene-encapsulated ordered aggregates of Fe3O4nanoparticles with nearly-spherical geometry and hollow interior were synthesized by a simple self-assembly process. We combine the unique properties of graphene sheets and a hollow assembly of nanoparticles to simultaneously provide a large reversible Li+storage capacity, good rate performance and long cycle life. A simple self-assembly process driven by electrostatic interaction was used to generate graphene-encapsulated hollow Fe3O4nanoparticle aggregates (G-HM, short for graphene-encapsulated hollow magnetite particles). In this process, graphene oxide and HM nanoparticle aggregates were first modified to acquire negative and positive charged respectively. The assembly was carried out under very mild reaction conditions and consequently perturbations to the intrinsic properties of the HM nanoparticles could be kept to a minimum. The G-HM composite particles synthesized as such showed remarkable cycle stability as well as lithium storage performance compared to the pristine HM nanoparticles or a mixture of graphene and HM particles. The graphene modification of porous nanoparticle aggregates is therefore a viable and facile approach to prepare high performance anode materials for the lithium ion batteries.
(6) We report a facile approach to fabricate monodisperse hollow porous Si (HPSi) nanoparticles (～120nm) via the magnesiothermic reduction of hollow porous SiO2(HPSiO2) nanoparticles formed by a templating method. This is followed by Ag nanoparticle coating for conductivity enhancement. The HPSi anode prepared as such shows several desirable electrochemical features:a high specific reversible capacity (3762mAh g-1), good cycle stability (>93%capacity retention after99cycles), and good rate performance (>2000mAh g-1at4000mA g-1), surpassing the performance of anode materials based on micron size macroporous Si particles.
引文
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