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1.
采用化学还原法,以抗坏血酸为还原剂,明胶为分散剂,将硝酸银溶液滴加到还原性溶液中制备电子材料用球形高纯超细银粉。探讨了还原过程中各种因素如硝酸银溶液浓度、分散剂、反应温度、搅拌速度等对银粉粒度大小及分布的影响。采用TEM、SEM对所得银粉进行了表征。  相似文献   

2.
以抗坏血酸为还原剂,在水溶液中还原银的前驱物制备超细银粉。考察了前驱物和分散剂种类以及分散剂用量对银粉颗粒形貌的影响。通过X射线衍射仪(XRD)和扫描电子显微镜(SEM)对银粉产品进行结构及形貌表征。结果表明:以硝酸银和银氨溶液为前驱物,随着PVP加入量的改变,银粉颗粒由树枝状向球形状转变,PVP加入量为30%时,制备出的银粉颗粒分散性好,球形度高,颗粒粒径为0.94μm。  相似文献   

3.
以硝酸银为反应原料,柠檬酸钠为还原剂,聚乙烯吡咯烷酮为保护剂,用水热法制备出纳米银颗粒。通过研究在柠檬酸钠不同浓度的条件下,对纳米银形貌形成的影响,从而达到还原剂浓度的优选。利用透射电子显微镜等对实验所得纳米银的结构形态及稳定性等进行表征。实验结果表明在AgNO_3浓度为0.1 mol/L,PVP为10 mg/mL,柠檬酸钠为0.15 mol/L,反应温度为100℃,反应时间为2 h的条件下可得到平均粒径约30 nm、分散性良好、尺寸均一的近球形纳米银颗粒。  相似文献   

4.
通过提取实验室废定影液中的银,采用化学还原法,分别以还原糖溶液、聚乙二醇(PEG)、三乙醇胺(TEA)为还原剂,制备超细银粉,对还原机理进行了分析,探讨了还原剂种类、溶液浓度、反应温度、反应物比例等对银粉形态及粒度大小的影响,采用X射线衍射仪(XRD)对所得样品物像结构进行了表征。结果表明,以三乙醇胺做还原剂可以制得高纯超细银粉。  相似文献   

5.
以氯化镁、氢氧化钠为原料,采用均相沉淀法制备超细氢氧化镁.研究了分散剂种类对氢氧化镁产率和粒径的影响,以及分散剂种类、氯化镁浓度、反应温度等因素对氢氧化镁沉降速率的影响,同时分别选择水、乙醇两种不同的反应介质,对氢氧化镁的粒径及产率进行对比.结果表明,以葡萄糖作为分散剂,氯化镁浓度为0.75 mol/L,反应温度为60℃,所得氢氧化镁产率较高,且粒径较小(约为6.4 μm)、粒度分布较均匀.  相似文献   

6.
以微反应器为核心反应设备,以硫酸镍为主要原料,水合肼和硼氢化钠为混合还原剂,非离子表面活性剂PVPK-30为分散剂,反应体系p H为11的条件下,控制反应温度为80℃,反应物Ni2+浓度为0.75mol/L,发生超声强化微反应,并辅以带搅拌的超声清洗装置清洗,磁力吸附装置收集,真空干燥箱干燥等过程,可制备得粒径为100nm左右、形貌为球形、尺寸分布窄的纳米镍粉。通过对新型微反应器、混合还原剂、镍离子初始浓度、反应温度等的研究,研究采用此种超声强化微反应法对制备纳米镍粉的粒径及形貌的影响。  相似文献   

7.
非水溶剂法制备纳米铜粉   总被引:1,自引:0,他引:1  
研究了以甘油作为还原剂,聚乙烯吡咯烷酮(PVP)作为分散剂,在液相甘油体系中还原醋酸铜(或氧化铜、氢氧化铜)制备纳米铜粉的方法。通过实验探索得到了最佳制备工艺条件:50 mL甘油体系中加入适量铜盐并使铜盐和甘油的物质的量比达到1∶40、同时加入分散剂PVP 0.4~0.6 g,控制温度为475~505 K,快速搅拌反应50~60 m in。所得产物通过化学分析,粉末X射线衍射(XRD)、透射电镜(TEM)表征,结果表明产物铜粉纯度比较高,粒径符合纳米材料的要求,并且粒子呈球型分布。  相似文献   

8.
本文采用碳热还原法,在氩气气氛下1750 ℃保温1 h制备出HfB2粉体,反应物HfO2、B2O3和C的物质的量比为1∶ 1∶ 10,其中HfO2以凝胶形式加入, HfO2凝胶通过NaBH4滴定HfCl4溶液制备,C分别以活性炭和碳纤维形式加入,聚乙二醇(PEG)作分散剂,乙醇作为混合介质.用XRD、SEM和EDS分析方法对所得粉体进行了表征.结果表明:用活性炭作为还原剂制备HfB2,颗粒细小,均匀,平均粒径5 μm,粒子为球形;用碳纤维作为还原剂制备HfB2,由于碳纤维活性差,反应不彻底,且碳纤维对颗粒形貌无影响.  相似文献   

9.
不同粒度的纳米碳酸钙具有不同的特性和应用范围,目前不同粒度纳米碳酸钙的可控制备方法还未见报道。以氯化钙、碳酸铵为原料,以乙醇、柠檬酸和焦磷酸钠为分散剂,采用复分解法研究了不同制备条件对纳米碳酸钙粒径的影响规律,在此基础上制备出平均粒径为17~71 nm的碳酸钙,并对其进行了表征。实验结果表明,所制备的纳米碳酸钙均为球霰石型,纯度很高,而且形貌近似球形。制备条件对纳米碳酸钙的粒径有显著的影响:随着反应温度升高,纳米碳酸钙的粒径减小;随着氯化钙滴加时间的增加,纳米碳酸钙的粒径增大;随着反应物浓度的提高,纳米碳酸钙的粒径先减小后增大;当分散剂为柠檬酸和焦磷酸钠的混合溶液时所得纳米碳酸钙的粒径最小,当分散剂为乙醇和焦磷酸钠的混合溶液时所得纳米碳酸钙的粒径最大。利用这些影响规律通过控制制备条件可以实现所需粒径纳米碳酸钙的可控制备。  相似文献   

10.
次磷酸盐液相还原法快速制备纳米银粉   总被引:16,自引:0,他引:16  
顾大明  高农  程谨宁 《精细化工》2002,19(11):634-635,674
以次磷酸钠为还原剂、六偏磷酸钠为分散剂、聚乙烯吡咯烷酮 (PVP)为保护剂 ,在 pH =1~ 2、温度为 4 0~ 4 2℃条件下与硝酸银溶液反应 ,得到紫红色银胶。经离心 (6 0 0 0r/min)分离、钝化剂溶液洗涤、真空干燥 (1× 10 3 Pa ,5 0℃ ) 3h ,得粉末状产物。透射电镜和X射线衍射仪分析表明 ,产品系粒径为 10~ 30nm纯相纳米银粉。本方法的制备周期约为 5h ,产率可达 70 %~80 %。  相似文献   

11.
鼓氧氰化法生产高纯度氰化银钾的研究   总被引:2,自引:0,他引:2  
以电解银粉为原料,采用鼓氧氰化法合成了氰化银钾,保持金属银过量投料,控制氰化银钾溶液浓缩水量是得到高纯度和高收率产品的关键,此方法具有原料简单,产吕纯度高,生产操作容易,生产成本低和环保要求低的优点,适合中小企业生产。  相似文献   

12.
The rapid and green formation of spherical and dendritic silver nanostructures based on microwave irradiation time was investigated. Silver nanoparticles were successfully fabricated by reduction of Ag(+) in a water medium and using polyvinylpyrrolidone (PVP) as the stabilizing agent and without the use of any other reducing agent, and were compared with those synthesized by conventional heating method. UV-vis absorption spectrometry, transmission electron microscopy (TEM), atomic absorption spectroscopy (AAS) and photon correlation spectroscopy (PCS) measurements, indicated that increasing the irradiation time enhanced the concentration of silver nanoparticles and slightly increased the particle size. There was a lack of large silver nanoparticles at a high concentration, but interestingly, the formation and growth of silver dendrite nanostructures appeared. Compared to conventional heating methods, the silver nanoparticle suspension produced by irradiated microwaves was more stable over a six-month period in aqueous solution without any signs of precipitation.  相似文献   

13.
Silver nanoparticles were produced by a chemical reduction method that reduced silver nitrate with reducing agents such as hydrazine and glucose. The silver nanoparticles were characterized with transmission electron microscope, scanning electron microscope, and optical microscope. The effects of process parameters such as the stirring speed, temperature, type of reducing agent, and dispersing agent on the particle size were studied. The particle size decreased with an increase in the stirring speed and a decrease in the process temperature. Smaller particles were formed when the silver nitrate was reduced by glucose versus those that were formed by reduction with hydrazine. Silver nanoparticles with average sizes of 10 and 35 nm, produced by reduction with hydrazine at 5 and 40°C, were applied to silk by an exhaust method. Silk fabrics treated with 40 ppm silver hydrosol produced at 5°C and 60 ppm silver hydrosol produced at 40°C showed 100% antimicrobial activity against the gram‐positive bacterium Staphylococcus aureus. The durability of the antimicrobial property of the treated silk fabric to washing was also examined and is presented. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008  相似文献   

14.
To prevent the evident agglomeration of silver nanoparticles during processing, this study reduced silver nanoparticles in pseudo-thermoplastic polyvinyl alcohol (PT-PVA) water solutions using the synchronous chemical reduction method. The PT-PVA coating could protect the silver nanoparticles to avoid agglomeration, allowing the silver nanoparticles to disperse uniformly in the PT-PVA. According to the particle size, TEM and UV-Vis analyses, the reduction of silver nanoparticles in PT-PVA solutions produced silver nanoparticles/PT-PVA films that had small particle size without agglomeration. Conversely, silver nanoparticles were added directly into PT-PVA, tended to have obvious agglomeration during the preparation process.  相似文献   

15.
Attempts to produce colloidal platinum nanoparticles by using steady absorption spectra with various chemical-based reduction methods often resulted in the fast disappearance of the absorption maxima leaving reduced platinum nanoparticles with little information on their optical properties. We synthesized colloidal platinum nanoparticles in an aqueous solution of polyvinyl pyrrolidone by gamma radiolytic reduction method, which produced steady absorption spectra of fully reduced and highly pure platinum nanoparticles free from by-product impurities or reducing agent contamination. The average particle size was found to be in the range of 3.4–5.3 nm and decreased with increasing dose due to the domination of nucleation over ion association in the formation of metal nanoparticles by the gamma radiolytic reduction method. The platinum nanoparticles exhibit optical absorption spectra with two absorption peaks centered at about 216 and 264 nm and the peaks blue shifted to lower wavelengths with decreasing particle size. The absorption spectra of platinum nanoparticles were also calculated using quantum mechanical treatment and coincidently a good agreement was obtained between the calculated and measured absorption peaks at various particle sizes. This indicates that the 216 and 264-nm absorption peaks of platinum nanoparticles conceivably originated from the intra-band transitions of conduction electrons of (n = 5, l = 2) and (n = 6, l = 0) energy states respectively to higher energy states. The absorption energies, i.e., conduction band energies of platinum nanoparticles derived from the absorption peaks increased with increasing dose and decreased with increasing particle size.  相似文献   

16.
The goal of the present study was to investigate the toxicity of biologically prepared small size of silver nanoparticles in human lung epithelial adenocarcinoma cells A549. Herein, we describe a facile method for the synthesis of silver nanoparticles by treating the supernatant from a culture of Escherichia coli with silver nitrate. The formation of silver nanoparticles was characterized using various analytical techniques. The results from UV-visible (UV-vis) spectroscopy and X-ray diffraction analysis show a characteristic strong resonance centered at 420 nm and a single crystalline nature, respectively. Fourier transform infrared spectroscopy confirmed the possible bio-molecules responsible for the reduction of silver from silver nitrate into nanoparticles. The particle size analyzer and transmission electron microscopy results suggest that silver nanoparticles are spherical in shape with an average diameter of 15 nm. The results derived from in vitro studies showed a concentration-dependent decrease in cell viability when A549 cells were exposed to silver nanoparticles. This decrease in cell viability corresponded to increased leakage of lactate dehydrogenase (LDH), increased intracellular reactive oxygen species generation (ROS), and decreased mitochondrial transmembrane potential (MTP). Furthermore, uptake and intracellular localization of silver nanoparticles were observed and were accompanied by accumulation of autophagosomes and autolysosomes in A549 cells. The results indicate that silver nanoparticles play a significant role in apoptosis. Interestingly, biologically synthesized silver nanoparticles showed more potent cytotoxicity at the concentrations tested compared to that shown by chemically synthesized silver nanoparticles. Therefore, our results demonstrated that human lung epithelial A549 cells could provide a valuable model to assess the cytotoxicity of silver nanoparticles.  相似文献   

17.
Continuous synthesis of silver nanoparticles based on a polyol process was conducted using a microwave-assisted flow reactor installed in a cylindrical resonance cavity. Silver nitrate (AgNO(3)) and poly(N-vinylpyrrolidone) (PVP) dissolved in ethylene glycol were used respectively as a silver metal precursor and as a capping agent of nanoparticles. Ethylene glycol worked as the solvent and simultaneously as the reductant. Silver nanoparticles of narrow size distributions were synthesized steadily for 5 h, maintaining almost constant yield (>93%) and quality. The reaction was achieved within 2.8 s of residence time, although nanoparticles were not formed under this flow rate by conventional heating. A narrower particle size distribution was realized by the increased flow rate of the reaction solution. Nanoparticles of 9.8 nm average size with a standard deviation of 0.9 nm were synthesized at the rate of 100 ml h(-l).  相似文献   

18.
马园园  寇伟  丁国生  徐联宾 《化工进展》2019,38(9):4191-4196
采用改进的Hummers法制备了氧化石墨烯(GO),然后以水合肼作为还原剂,并控制反应的pH=10来制备还原氧化石墨烯(RGO)。采用化学还原法,以石墨烯为载体,以乙酰丙酮银为前体,以硼氢化锂四氢呋喃溶液为还原剂将银离子还原,制备了石墨烯负载纳米银复合材料。通过X 射线粉末衍射(XRD)、傅里叶变换红外光谱(FTIR)和透射电子显微镜(TEM)等表征方法证明了石墨烯上负载的银纳米颗粒结晶良好、尺寸均一、分布均匀,其中银纳米颗粒直径约为8nm。通过循环伏安和计时电流技术对石墨烯负载纳米银复合材料进行电化学测试,结果表明,石墨烯负载纳米银复合材料对过氧化氢的还原具有良好的电催化活性。以此复合纳米结构构建的过氧化氢传感器测试过氧化氢浓度的线性范围为0.1~62.3mmol/L(R=0.990),检出限为0.017mmol/L(S/N=3),响应时间小于2s。  相似文献   

19.
Silver/polyaniline (Ag-PANi) nanocomposites were prepared via in situ reduction of silver in aniline by mild photolysis performed with short wavelength (365 nm) radiation from UV lamp for 12 h. Reduction of the silver in aqueous aniline leads to the formation of silver nanoparticles which in turn catalyze oxidation of aniline into polyaniline. A slightly broadened X-ray diffraction (XRD) pattern suggests small particle which was size consistent with cubic silver nanoparticles. The UV–Vis absorption revealed that the bands at about 400–420 nm due to benzonoid ring of the polyaniline are overlapped and blue-shifted due to the presence of silver nanoparticles in powdered state. Scanning electron microscopy (SEM) of the silver/polyaniline (Ag-PANi) nanocomposite showed a size distribution with nanofibers and granular morphology of silver nanoparticles. Our findings are not only the promising approach for electro-catalytic hydrazine oxidation but also utilized in the other bio-sensing applications.  相似文献   

20.
Four Ru nanoparticles of different mean sizes from 1.13 to 17.22 nm were prepared and used as catalysts for the selective hydrogenation of polyunsaturated soybean oil at 353 K and initial pressure of 1.5 MPa. The catalyst with the smallest mean size (1.13 nm) had the lowest activity, the activity increased as the mean size increased to 3.10 nm, then decreased with further increase in the mean particle size. The cistrans isomerization rate decreased with the increase in particle size.  相似文献   

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