首页 | 本学科首页   官方微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   2917篇
  免费   830篇
  国内免费   430篇
化学   1500篇
晶体学   47篇
力学   178篇
综合类   44篇
数学   285篇
物理学   2123篇
  2024年   8篇
  2023年   52篇
  2022年   85篇
  2021年   78篇
  2020年   84篇
  2019年   77篇
  2018年   104篇
  2017年   146篇
  2016年   133篇
  2015年   139篇
  2014年   255篇
  2013年   227篇
  2012年   250篇
  2011年   277篇
  2010年   214篇
  2009年   200篇
  2008年   205篇
  2007年   234篇
  2006年   197篇
  2005年   193篇
  2004年   145篇
  2003年   136篇
  2002年   91篇
  2001年   84篇
  2000年   63篇
  1999年   51篇
  1998年   53篇
  1997年   55篇
  1996年   48篇
  1995年   51篇
  1994年   37篇
  1993年   24篇
  1992年   33篇
  1991年   19篇
  1990年   19篇
  1989年   14篇
  1988年   9篇
  1987年   15篇
  1986年   9篇
  1985年   14篇
  1984年   11篇
  1983年   9篇
  1982年   14篇
  1981年   6篇
  1980年   1篇
  1979年   2篇
  1978年   2篇
  1977年   2篇
  1976年   1篇
  1975年   1篇
排序方式: 共有4177条查询结果,搜索用时 15 毫秒
31.
聚多巴胺还原高锰酸钾制备二氧化锰阵列纳米管   总被引:1,自引:1,他引:0  
以通过水热法在石英玻璃片表面合成的ZnO纳米棒为模板,在其表面生成聚多巴胺薄膜,然后与KMnO4反应,制备了MnO_2阵列纳米管。经表征发现,制备的MnO_2纳米管形态良好,在基底表面的附着力强;所制备的MnO_2为非晶型。由于ZnO模板易合成、易去除、形态好,且聚多巴胺薄膜的生成方法也很简便易行,使得该制备MnO_2纳米管阵列的方法具有简便、快捷、适用性广等的特性,对MnO_2新形态纳米结构的构建具有一定的启示作用。  相似文献   
32.
采用超声提取的方式,以离子色谱法测定土壤易溶盐中的氯离子和硫酸根离子。对实验条件进行了优化,色谱柱为NJ–SA–4A柱(250 mm×2 mm),保护柱为SI–92G柱(50 mm×4 mm),淋洗液为1.8 mmol/L Na_2CO_3–1.7mmol/L NaHCO_3,流量为1.0 m L/min;在40℃下,对土壤样品提取10 min。Cl~–和SO_4~(2–)在检测范围内均线性良好,线性相关系数为0.999 8,加标回收率分别为95.0%~99.0%,96.0%~101.0%,测定结果的相对标准偏差分别为1.4%,1.0%(n=4)。与传统的方法相比,该法试剂用量少,操作简单,可用于土壤易溶盐样品的测定。  相似文献   
33.
Orthogonal array design was used to optimize arsenic speciation in drinking water in contact with materials by dispersive liquid–liquid microextraction followed by graphite furnace atomic absorption spectrometry. Arsenic speciation was achieved by the formation of an arsenic(III) hydrophobic complex with a new chelating agent, 1,2,6-hexanetriol trithioglycolate, at neutral pH. The complex was extracted into the organic phase, while arsenic(V) remained in aqueous solution. The concentration of As(V) was determined by subtracting As(III) from the total arsenic following the reduction of As(V) to As(III) by L-cysteine. Orthogonal array design with OA16 (44) and OA9 (33) matrices was used to optimize the efficiency of dispersive liquid–liquid microextraction and the reduction of As(V) to As(III), respectively. Under the optimal conditions, the detection limit was 0.03?µg?L?1 for As(III) and the relative standard deviation was 5.9% with an enhancement factor of 87. The calibration curve was linear from 0.19 to 3.0?µg?L?1 with a correlation coefficient of 0.9996. The developed method was used for arsenic speciation in solutions of drinking water that contacted materials. The recoveries of fortified samples were in an acceptable range from 92.0 to 113.3%.  相似文献   
34.
Historical textiles in the Topkap? Museum, which are called silk kaftans and brocades by art historians from the sixteenth and nineteenth were characterized by scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM–EDX) and high-performance liquid chromatography with diode array detection for identification of metal threads and dyestuffs. In the most Ottoman textiles, metal threads, especially belonging to the sultans, were used as the gold gild. Although the chemical composition of the samples on the surface may easily be obtained by SEM–EDX, the thickness of the thin gold layer on metal threads cannot be obtained directly. Hence, the goal of this project is to describe whether metal threads are gilded or not and to measure coating thickness. A new method was developed for measuring the thickness of gold layer, and the modeling was reformed. The SEM–EDX results were interpreted in accordance with the theoretical models. The coating thickness of metal threads was subsequently measured in ancient textiles. The thickness, depth, and valuable metal composition in the threads of the artistic objects were obtained by this approach. Dye analysis was used to characterize the presence of indigotin, carminic acid, ellagic acid, and luteolin in the historical textiles.  相似文献   
35.
Well‐oriented ZnO nanorods (NRs) arrays were grown on Si, alumina, quartz, and FTO substrates through a ZnO seed layer followed by low temperature wet chemical process. The influence of sputtered ZnO seed layer thickness (100, 50, 32, and 16 nm), annealing temperature and CuOx coverage on the characteristics of ZnO NRs were investigated in this study. The crystalline structural, chemical, morphological, optical, and electrical properties of ZnO NRs arrays were studied by X‐ray diffraction (XRD), field emission‐ scanning electron microscopy equipped by energy dispersive X‐ray spectroscopy (FE‐SEM/EDX), Raman scattering, UV/Vis ‐ near IR absorption spectroscopy and current‐voltage characteristic. XRD and Raman spectra measurement revealed that the synthesize ZnO displayed hexagonal wurtzite structure. The individual rod diameter, density, and orientation can be controlled by varying the seed layer thickness. The mean diameter and maximum length of ZnO NRs are around 55–66 nm and 282 nm, respectively. ZnO NRs/ ZnO thin film structure shows optical switching and negative differential resistance behavior as applicable to ON/OFF gate and memory devices.  相似文献   
36.
In this paper, effect of emulsification processes on the properties of Pickering emulsions stabilized by organomontmorillonites (OMts) was studied. Results of micro-morphology and X-ray diffraction showed that the structure of OMt in emulsion depended on the emulsification processes and had an effect on the stability of emulsion. We propose a schematic diagram to reveal the relationship between emulsification processes-OMt laminates structure-stability of Pickering emulsion. In emulsion prepared by ultrasonic, OMt showed uniform dispersion, loose structure, and irregular crystalline. In emulsion prepared by vortex mixing method, OMt illustrated stacking and coagulation structure. In emulsion prepared by microwave method, OMt showed interacting structure and had a little interaction with oil/water interface, and thus the properties of emulsion prepared by microwave was weakly related to oil/water ratios. Emulsification processes had a profound effect on the structure of OMt and stability of Pickering emulsion, which can be used as a trigger to prepare emulsion for various applications.  相似文献   
37.
Psoraleae Fructus is one of the most popular traditional Chinese medicines. Coumarins, flavonoids, and meroterpenes are the main contributors to the biological activity of Psoraleae Fructus. In this study, a new method for the quality control of Psoraleae Fructus was developed, through the quantitative analysis of multicomponents by single marker with diode array detector. Thirteen components, including psoralenoside, isopsoralenoside, psoralen, isopsoralen, psoralidin, neobavaisoflavone, bavachin, corylin, isobavachalcone, corylifol A, bavachinin, bavachalcone, and bakuchiol were rapidly separated and identified within 12 min by the newly developed method. The feasibility and reliability of this method were corroborated. The method was also compared to the external standard method and detection by corona charged aerosol detector. The results of percent difference (%) and cos (θ) have shown that there were no significant differences observed between the quantitative analysis of multicomponents by single marker and external standard method analyses; psoralen and isopsoralen were undetectable with the corona charged aerosol detector due to their but the sensitivity for all the compounds except bakuchiol detected by corona charged aerosol detector are higher than those obtained by diode array detector. In addition, the newly method developed was applied to the quality evaluation of Chinese patent medicines containing Psoraleae Fructus.  相似文献   
38.
Spices are a popular food of plant origin, rich in various phytochemicals and recognized for their numerous properties. The aim of the study was to evaluate the antioxidant and antimicrobial activity, as well as the content of specialized metabolites, of aqueous extracts of three spice species––garlic (Allium sativum L.), ginger (Zingiber officinalle L.) and turmeric (Curcuma longa L.)––prepared by green extraction methods. Ultrasound treatment increased the chromaticity parameter b value of turmeric and ginger extracts, thus indicating a higher yellow color predominantly due to curcuminoids characteristic of these species. Ultrasound-assisted extraction significantly increased the content of total soluble solids, phenolic compounds, total carotenoids and vitamin C. The temperature of the system was also an important factor, with the highest (70 °C) conditions in ultrasound-assisted extraction having a positive effect on thermolabile compounds (vitamin C, phenolics, total carotenoids). For example, turmeric extract treated with ultrasound at 70 °C had up to a 67% higher vitamin C content and a 69.4% higher total carotenoid content compared to samples treated conventionally at the same temperature, while ginger extracts had up to 40% higher total phenols. All different concentrations of spice extracts were not sufficient for complete inhibition of pathogenic bacterial strains of Salmonella, L. monocytogenes and S. aureus; however, only garlic extracts had an effect on slowing down the growth and number of L. monocytogenes colonies. Spice extracts obtained by ultrasonic treatment contained a significantly higher level of bioactive compounds and antioxidant capacity, suggesting that the extracts obtained have significant nutritional potential and thus a significant possibility for phytotherapeutic uses.  相似文献   
39.
采用模压成型方法制备了2种柔软性不同的热塑性聚氨酯/短切碳纤维/碳纳米管(TPU/SCF-CNT)复合材料复制物, 其表面上具有倒金字塔微结构阵列, 内部有SCF与CNT共同构成的导电通路. 将复合材料复制物和相应的复合材料平整片封装成柔性传感器. 结果表明, 压力作用下传感器内复制物和平整片之间的接触电阻因倒金字塔底棱的形变而显著降低. 对使用柔软性较高的复合材料封装的传感器, 虽然其相对迟滞稍大, 但压力作用下倒金字塔底棱形变量较大, 且复制物和平整片内导电通路增加量较大, 因此其在0~2.5 kPa的线性区内具有较高的灵敏度(0.32 kPa?1). 制备的2种传感器均具有快速响应特性, 且能在500 s(约1580次)的循环压缩/释放测试(峰值压力约3 kPa)中保持较稳定的电阻响应. 研究表明, 利用模压成型的表面倒金字塔结构复合材料复制物封装成的柔性压力传感器具有良好的传感性能.  相似文献   
40.
王许欣  周澍堃  李晓敏  张庆合 《色谱》2021,39(6):652-658
福美双是重要的二硫代氨基甲酸酯(DTC)杀菌剂,在小麦中使用限量以1 mg/kg二硫化碳(CS2)计。目前我国相关检测方法是针对二硫代氨基甲酸酯一类的化合物,二硫代氨基甲酸酯通过与酸反应生成CS2,采用光谱法或色谱法测定CS2,间接实现二硫代氨基甲酸酯测定。该方法无法特异性实现对福美双的检测,因此开展小麦粉中福美双检测方法的研究具有重要意义。研究建立了高效液相色谱-二极管阵列检测(HPLC-DAD)测定小麦粉及面粉改良剂中福美双的分析方法。小麦粉及面粉改良剂样品用乙腈溶剂提取后,经涡旋、振荡、冰水浴超声和静置后取上清液过滤,供高效液相色谱测定。采用ZORBAX plus-C18色谱柱(150 mm×4.6 mm, 5 μm)分离,以水-乙腈为流动相洗脱分析,在波长280 nm下检测。实验优化了提取溶剂及其体积、振荡超声条件、色谱柱、检测波长、流动相等条件。该方法采用保留时间和紫外光谱图定性,外标法定量。该方法在线性范围内(0.30~30.0 μg/mL)线性关系良好,相关系数(r2)为0.99999。对小麦粉及面粉改良剂进行1.5、3.0、15 mg/kg 3个水平的加标回收试验,福美双的回收率为89.6%~98.3%,相对标准偏差为1.6%~3.9%(n=6)。方法的检出限和定量限分别为0.5 mg/kg和1.5 mg/kg。该方法采用溶剂提取,操作简单,分析时间短,特异性好,具有精密度高、重复性好、检出限低等特点,适用于小麦粉及面粉改良剂中福美双快速、准确的定量检测。  相似文献   
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号