纳米银胶及载银蒙脱石的制备与抗菌性能
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摘要
银纳米粒子已经被广泛地用在摄影、催化、生物传感器、光子学、光电子学、表面增强拉曼散射检测和抗菌等领域。许多研究已证实纳米银的性能与其尺寸、尺寸分布和形貌等因素密切相关，因此如何控制纳米银的形核与生长从而获得具有特定优异性能的纳米银的研究是目前的热点之一。在微生物对传统抗生素耐药性日渐增强的今天，开展对具有强烈的广谱抗菌活性且不易产生耐药性的纳米银的研究有着重大的现实意义。本文回顾了银系抗菌材料的研究进展，分别介绍了银离子和纳米银的抗菌机理，阐述了纳米银抗菌活性具有形貌、尺寸和尺寸分布依赖性。银粒子的尺寸越小、分布越均匀，其抗菌活性越强。然后，就如何简单、快速、绿色合成小粒径且分布均匀的银纳米粒子进行了详细探讨。主要内容如下：
分别以AgNO_3、[Ag(NH_3)_2]NO_3(AgNO_3与NH_3·H_2O反应)、不含NO_3~-离子的银盐与NH_3·H_2O反应制备的[Ag(NH_3)_2]~+络合离子水溶液为前驱体，以聚乙烯吡咯烷酮(PVP)兼作还原剂和稳定剂，再加入少量的添加剂，通过紫外光还原法制备纳米银溶胶。紫外-可见光谱和透射电子显微镜分析表明：以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体反应速率最快、粒径最小、分布最均匀、稳定性最好；[Ag(NH_3)_2]NO_3水溶液次之；AgNO_3水溶液最差。此外，以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体，考察了PVP浓度、温度和pH值对形成的纳米银溶胶影响。结果表明：纳米银的形核速率随温度、PVP浓度的增大而增大，但当PVP／Ag~+离子的质量比超过10：1时，反应速率变化不明显，因此以PVP与Ag~+离子的质量比为10：1最好；当前驱体的pH值为12．68时，纳米银的形核速率最快，而当pH值小于或者大于12．68时，形核速率较小。在PVP／Ag~+为10：1，pH值为12．68条件下，通过紫外光还原法制备的纳米银粒子的粒径为1-3nm的球形银粒子，室温下避光存放三个月，未出现任何絮凝或者沉淀现象。
前驱体、还原剂及添加剂的种类同上，通过微波辐射还原法制备纳米银溶胶。考察了前驱体种类、PVP浓度、微波功率、pH值等因素对形成的纳米银溶胶的影响。结果表明：以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体、PVP／Ag~+为8：1(质量比)、pH值为12．4、微波辐射功率为中低火时，Ag~+离子的转化率最高，所得银纳米粒子的粒径小、单分散且稳定性好。
以两高纯银片做电极，以去离子水为电解液，PVP作为辅助电解质和稳定剂，通过电解法制备高纯纳米银溶胶。探讨了PVP含量、电解时间、电流密度对形成的纳米银溶胶的影响。结果表明：当PVP含量为5％、电解150min、电流密度为1-2mA／cm~2时，所得球形银粒子的粒径约1．3nm左右、单分散，而且有极好的存放稳定性，室温避光存放6个月无任何可见的变化。
分别以AgNO_3、不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液与钠基蒙脱石(Na-MMT)在60℃进行离子交换，然后，加入一定量的PVP兼作还原剂和稳定剂，再加入少量的添加剂，通过微波辐射还原法制备了Ag-MMT。用X-射线衍射(XRD)测定了Na-MMT及Ag-MMT的结构，MMT的片层间距减小表明Ag~+离子或者Ag(NH_3)_2]~+络合离子与Na-MMT中的Na~+、K~+等发生了交换。用场发射扫描电子显微镜(FE-SEM)表征了Ag-MMT负载的银粒子的大小、形貌，表明银纳米粒子是球形的，粒径20-30nm左右。用X-射线荧光探针(XRF)分析了Ag-MMT样品中的银含量。用热重分析(TGA)对Na-MMT及Ag-MMT的热稳定性进行了表征，结果表明经[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT有更好的热稳定性。
分别以大肠杆菌(E．coli)和金黄色葡萄球菌(S．aureus)为代表，研究了纳米银溶胶、Na-MMT和Ag-MMT的抗菌性能。结果显示无论通过紫外光辐射法、微波法还是通过电解法制备的纳米银溶胶的最小抑菌浓度(MIC)均为1．25ppm，最小杀菌浓度(MBC)均为2．0ppm，杀菌率均超过了99．9％。Na-MMT无抗菌活性，由AgNO_3和[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT的MIC分别为100ppm、150ppm，两者的杀菌率均超过了99．9％，但经[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT中的银有更好的缓释性能。用所制备的纳米银溶胶分别处理纱布、层压地板和木板膜，当所用纳米银溶胶的浓度达到20ppm时，产品的杀菌率都均超过了99．9％。
Silver nanoparticles of stable dispersions have been used mostly in areas such asphotography, catalysis, biosensor, photonics, optoelectronics, surface-enhanced Ramanscattering (SERS) detection and antibacterial. Many studies have demonstrated a closerelation between the properties of silver nanoparticles and their sizes, shapes and sizedistributions. Thus, to tailor silver nanoparticles with novel properties, it has been one offocuses that how to control deliberately the nucleation and growth of silver nanoparticles.Nowadays, microbes have a stronger and stronger resistance to traditional antibiotic, so ithas great practical significance to study nano-silver with a strong, broad-spectrumantibacterial activity and difficult to generate resistance. The development of silverantimicrobial materials was reviewed, and the antimicrobial mechanisms of nano-silverand silver ions were introduced, respectively. The antibacterial property of nano-silverdepened on morpholopy, size and size distribution. The smaller for size and moreuniform for size distribution, the stronger the antibacterial activity of silver particles is.Then, it have been explored in detail on how to synthesize the silver nanoparticles withsmall size and uniform size distribution.by an easy, fast and green method. The workmainly includes the following aspects:
AgNO_3, [Ag(NH_3)_2]NO_3 and [Ag(NH_3)_2]~+ complex ion aqueous solutions withoutNO_3~- were used as precusors, and the colloidal silver nanoparticles were synthesized byUV irradiation of using poly(N-vinyl-2-pyrrolidone) (PVP) as both reducing andstabilizing agents after a little of additive was added, respectively,. The UV-Vis. spectraand transmission electron microscopy (TEM) showed that the nucleation rate of silvernanoparticles was the fastest, smallest in size and most uniform in size distribution andmost stable when [Ag(NH_3)_2]~+ complex ion aqueous solution without NO_3~- was used asprecursor; [Ag(NH_3)_2]NO_3, the second; and AgNO_3, the worst. In addition, the effects ofconcentration of PVP, temperature and pH value to the as-prepared silver sols were investigated using [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~- as precusor.The results indicated that the nucleation rate of silver nanoparticles increased withreaction temperature and concentration of PVP, however, the rate is almost unchangeablewhen the PVP/Ag~+ (weight ratio) was over 10:1. Therefore, it was the best weightratio 10:1 for PVP/Ag~+. The tests about the effects of pH values to the nucleation rate ofsilver nanoparticles showed the most appropriate pH value of the precursor solutions was12.68. The silver particles prepared in the most appropriate PVP/Ag~+ and pH value werespheric about 1-3 nm in diameter, and no flocculation or deposition appeared even if theywere placed in dark at room temperature for three months.
The colloidal silver nanoparticles were synthesized by microwave irradiationreduction method, and the precusors, reductants and additives were all the same as theabove. The effects of precusors, concentrations of PVP, microwave powers and pHvalues to the as-prepared nano-silver sols have been investigated. The results showed thatthe silver ions had the highest conversion ratio using [Ag(NH_3)_2]~+ complex ion aqueoussolutions without NO_3~- as precursor, 8:1 for PVP/Ag~+ (wt ratio), low middle fire formicrowave power and 12.4 for pH value, and the silver particles were about 1-3 nm insize, monodispersion and fine stability.
A highly pure nano-silver sols were prepared by electrolysis method using twohighly pure silver flakes as electrodes and deionized water as electrolytic solution, andPVP served as the supporting electrolyte and stabilizer. The effects of content of PVP,electrolytic time and current density to the colloidal silver nanoparticles were researched.The results indicated that as-synthesized particles were spherical about 1-3 nm in size,monodispersion under the condition of 5 wt % PVP with current density 1-2mA/cm~2 for150 min, moreover, the silver sol had such an excellent stability that it had not any changethough it was placed in dark at room temperature for six months.
The hydrated sodium ions in Na-montmorillonite (Na-MMT) lamellars wereexchanged at 60℃by AgNO_3 and [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~-, respectively. Then the Ag-MMTs were attained by microwave irradiation usingPVP as both reducing and stabilizing agents. The structures of Na-MMT and Ag-MMTswere characterized by XRD, and the distance between two lamellars decreased indicatedthat the exchange had happened between Ag~+ ions or [Ag(NH_3)_2]~+ complex ions andNa~+、K~+ in the lamellars of MMT. The size and morphology of silver particles loaded onthe surface of Ag-MMT were investigated by field emission scan electron microscope(FE-SEM), and results showed the silver particles were spherical about 20-30 nm in size.The Ag contents of the Na-MMT and the Ag-MMTs were analysed comparatively withX-ray Fluorescent probe. Thermogravimetry analysis showed the Ag-MMT had a morestability from [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~- than fromAgNO_3.
The antibacterial properties of nano-silver sols, Na-MMT and Ag-MMTs werestudied using E.coli and S.aureus as representative bacteria. The results showed that theminimal inhibitory concentrations (MIC) of nano-silver sols prepared either by UVphotoreduction, microwave irradiation or electrolysis method were all 1.25 ppm, minimalbactericidal concentrations (MBC) all 2.0 ppm, and bactericidal ratios were beyond 99.9%.The Na-MMT had not and antibacterial activity, and the MICs of Ag-MMTs prepared byAgNO_3 were 100 ppm and 150 ppm by [Ag(NH_3)_2]~+ complex ion, respectively. Both ofbactericidal ratios were beyond 99.9%. However, the Ag in the Ag-MMT had a betterslow release proterty from [Ag(NH_3)_2]~+ complex ion than from AgNO_3. The pledget,laminate wood flooring and boarding film were dealed with as-prepared nano-silver sols,respectively, and the bactericidal ratios of all the products were beyond 99.9% when theconcentrations of nano-silver sols were up to 20 ppm.
分别以AgNO_3、[Ag(NH_3)_2]NO_3(AgNO_3与NH_3·H_2O反应)、不含NO_3~-离子的银盐与NH_3·H_2O反应制备的[Ag(NH_3)_2]~+络合离子水溶液为前驱体，以聚乙烯吡咯烷酮(PVP)兼作还原剂和稳定剂，再加入少量的添加剂，通过紫外光还原法制备纳米银溶胶。紫外-可见光谱和透射电子显微镜分析表明：以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体反应速率最快、粒径最小、分布最均匀、稳定性最好；[Ag(NH_3)_2]NO_3水溶液次之；AgNO_3水溶液最差。此外，以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体，考察了PVP浓度、温度和pH值对形成的纳米银溶胶影响。结果表明：纳米银的形核速率随温度、PVP浓度的增大而增大，但当PVP／Ag~+离子的质量比超过10：1时，反应速率变化不明显，因此以PVP与Ag~+离子的质量比为10：1最好；当前驱体的pH值为12．68时，纳米银的形核速率最快，而当pH值小于或者大于12．68时，形核速率较小。在PVP／Ag~+为10：1，pH值为12．68条件下，通过紫外光还原法制备的纳米银粒子的粒径为1-3nm的球形银粒子，室温下避光存放三个月，未出现任何絮凝或者沉淀现象。
前驱体、还原剂及添加剂的种类同上，通过微波辐射还原法制备纳米银溶胶。考察了前驱体种类、PVP浓度、微波功率、pH值等因素对形成的纳米银溶胶的影响。结果表明：以不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液为前驱体、PVP／Ag~+为8：1(质量比)、pH值为12．4、微波辐射功率为中低火时，Ag~+离子的转化率最高，所得银纳米粒子的粒径小、单分散且稳定性好。
以两高纯银片做电极，以去离子水为电解液，PVP作为辅助电解质和稳定剂，通过电解法制备高纯纳米银溶胶。探讨了PVP含量、电解时间、电流密度对形成的纳米银溶胶的影响。结果表明：当PVP含量为5％、电解150min、电流密度为1-2mA／cm~2时，所得球形银粒子的粒径约1．3nm左右、单分散，而且有极好的存放稳定性，室温避光存放6个月无任何可见的变化。
分别以AgNO_3、不含NO_3~-离子的[Ag(NH_3)_2]~+络合离子水溶液与钠基蒙脱石(Na-MMT)在60℃进行离子交换，然后，加入一定量的PVP兼作还原剂和稳定剂，再加入少量的添加剂，通过微波辐射还原法制备了Ag-MMT。用X-射线衍射(XRD)测定了Na-MMT及Ag-MMT的结构，MMT的片层间距减小表明Ag~+离子或者Ag(NH_3)_2]~+络合离子与Na-MMT中的Na~+、K~+等发生了交换。用场发射扫描电子显微镜(FE-SEM)表征了Ag-MMT负载的银粒子的大小、形貌，表明银纳米粒子是球形的，粒径20-30nm左右。用X-射线荧光探针(XRF)分析了Ag-MMT样品中的银含量。用热重分析(TGA)对Na-MMT及Ag-MMT的热稳定性进行了表征，结果表明经[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT有更好的热稳定性。
分别以大肠杆菌(E．coli)和金黄色葡萄球菌(S．aureus)为代表，研究了纳米银溶胶、Na-MMT和Ag-MMT的抗菌性能。结果显示无论通过紫外光辐射法、微波法还是通过电解法制备的纳米银溶胶的最小抑菌浓度(MIC)均为1．25ppm，最小杀菌浓度(MBC)均为2．0ppm，杀菌率均超过了99．9％。Na-MMT无抗菌活性，由AgNO_3和[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT的MIC分别为100ppm、150ppm，两者的杀菌率均超过了99．9％，但经[Ag(NH_3)_2]~+络合离子水溶液处理得到的Ag-MMT中的银有更好的缓释性能。用所制备的纳米银溶胶分别处理纱布、层压地板和木板膜，当所用纳米银溶胶的浓度达到20ppm时，产品的杀菌率都均超过了99．9％。
Silver nanoparticles of stable dispersions have been used mostly in areas such asphotography, catalysis, biosensor, photonics, optoelectronics, surface-enhanced Ramanscattering (SERS) detection and antibacterial. Many studies have demonstrated a closerelation between the properties of silver nanoparticles and their sizes, shapes and sizedistributions. Thus, to tailor silver nanoparticles with novel properties, it has been one offocuses that how to control deliberately the nucleation and growth of silver nanoparticles.Nowadays, microbes have a stronger and stronger resistance to traditional antibiotic, so ithas great practical significance to study nano-silver with a strong, broad-spectrumantibacterial activity and difficult to generate resistance. The development of silverantimicrobial materials was reviewed, and the antimicrobial mechanisms of nano-silverand silver ions were introduced, respectively. The antibacterial property of nano-silverdepened on morpholopy, size and size distribution. The smaller for size and moreuniform for size distribution, the stronger the antibacterial activity of silver particles is.Then, it have been explored in detail on how to synthesize the silver nanoparticles withsmall size and uniform size distribution.by an easy, fast and green method. The workmainly includes the following aspects:
AgNO_3, [Ag(NH_3)_2]NO_3 and [Ag(NH_3)_2]~+ complex ion aqueous solutions withoutNO_3~- were used as precusors, and the colloidal silver nanoparticles were synthesized byUV irradiation of using poly(N-vinyl-2-pyrrolidone) (PVP) as both reducing andstabilizing agents after a little of additive was added, respectively,. The UV-Vis. spectraand transmission electron microscopy (TEM) showed that the nucleation rate of silvernanoparticles was the fastest, smallest in size and most uniform in size distribution andmost stable when [Ag(NH_3)_2]~+ complex ion aqueous solution without NO_3~- was used asprecursor; [Ag(NH_3)_2]NO_3, the second; and AgNO_3, the worst. In addition, the effects ofconcentration of PVP, temperature and pH value to the as-prepared silver sols were investigated using [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~- as precusor.The results indicated that the nucleation rate of silver nanoparticles increased withreaction temperature and concentration of PVP, however, the rate is almost unchangeablewhen the PVP/Ag~+ (weight ratio) was over 10:1. Therefore, it was the best weightratio 10:1 for PVP/Ag~+. The tests about the effects of pH values to the nucleation rate ofsilver nanoparticles showed the most appropriate pH value of the precursor solutions was12.68. The silver particles prepared in the most appropriate PVP/Ag~+ and pH value werespheric about 1-3 nm in diameter, and no flocculation or deposition appeared even if theywere placed in dark at room temperature for three months.
The colloidal silver nanoparticles were synthesized by microwave irradiationreduction method, and the precusors, reductants and additives were all the same as theabove. The effects of precusors, concentrations of PVP, microwave powers and pHvalues to the as-prepared nano-silver sols have been investigated. The results showed thatthe silver ions had the highest conversion ratio using [Ag(NH_3)_2]~+ complex ion aqueoussolutions without NO_3~- as precursor, 8:1 for PVP/Ag~+ (wt ratio), low middle fire formicrowave power and 12.4 for pH value, and the silver particles were about 1-3 nm insize, monodispersion and fine stability.
A highly pure nano-silver sols were prepared by electrolysis method using twohighly pure silver flakes as electrodes and deionized water as electrolytic solution, andPVP served as the supporting electrolyte and stabilizer. The effects of content of PVP,electrolytic time and current density to the colloidal silver nanoparticles were researched.The results indicated that as-synthesized particles were spherical about 1-3 nm in size,monodispersion under the condition of 5 wt % PVP with current density 1-2mA/cm~2 for150 min, moreover, the silver sol had such an excellent stability that it had not any changethough it was placed in dark at room temperature for six months.
The hydrated sodium ions in Na-montmorillonite (Na-MMT) lamellars wereexchanged at 60℃by AgNO_3 and [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~-, respectively. Then the Ag-MMTs were attained by microwave irradiation usingPVP as both reducing and stabilizing agents. The structures of Na-MMT and Ag-MMTswere characterized by XRD, and the distance between two lamellars decreased indicatedthat the exchange had happened between Ag~+ ions or [Ag(NH_3)_2]~+ complex ions andNa~+、K~+ in the lamellars of MMT. The size and morphology of silver particles loaded onthe surface of Ag-MMT were investigated by field emission scan electron microscope(FE-SEM), and results showed the silver particles were spherical about 20-30 nm in size.The Ag contents of the Na-MMT and the Ag-MMTs were analysed comparatively withX-ray Fluorescent probe. Thermogravimetry analysis showed the Ag-MMT had a morestability from [Ag(NH_3)_2]~+ complex ion aqueous solutions without NO_3~- than fromAgNO_3.
The antibacterial properties of nano-silver sols, Na-MMT and Ag-MMTs werestudied using E.coli and S.aureus as representative bacteria. The results showed that theminimal inhibitory concentrations (MIC) of nano-silver sols prepared either by UVphotoreduction, microwave irradiation or electrolysis method were all 1.25 ppm, minimalbactericidal concentrations (MBC) all 2.0 ppm, and bactericidal ratios were beyond 99.9%.The Na-MMT had not and antibacterial activity, and the MICs of Ag-MMTs prepared byAgNO_3 were 100 ppm and 150 ppm by [Ag(NH_3)_2]~+ complex ion, respectively. Both ofbactericidal ratios were beyond 99.9%. However, the Ag in the Ag-MMT had a betterslow release proterty from [Ag(NH_3)_2]~+ complex ion than from AgNO_3. The pledget,laminate wood flooring and boarding film were dealed with as-prepared nano-silver sols,respectively, and the bactericidal ratios of all the products were beyond 99.9% when theconcentrations of nano-silver sols were up to 20 ppm.
引文
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