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   3453篇
  免费   273篇
  国内免费   165篇
化学   823篇
晶体学   40篇
力学   190篇
综合类   3篇
数学   43篇
物理学   2792篇
  2024年   1篇
  2023年   20篇
  2022年   33篇
  2021年   36篇
  2020年   47篇
  2019年   39篇
  2018年   54篇
  2017年   98篇
  2016年   150篇
  2015年   108篇
  2014年   284篇
  2013年   234篇
  2012年   193篇
  2011年   254篇
  2010年   195篇
  2009年   226篇
  2008年   212篇
  2007年   263篇
  2006年   185篇
  2005年   166篇
  2004年   162篇
  2003年   113篇
  2002年   131篇
  2001年   134篇
  2000年   96篇
  1999年   100篇
  1998年   89篇
  1997年   59篇
  1996年   36篇
  1995年   28篇
  1994年   31篇
  1993年   23篇
  1992年   16篇
  1991年   20篇
  1990年   11篇
  1989年   5篇
  1988年   9篇
  1987年   7篇
  1986年   2篇
  1985年   1篇
  1984年   5篇
  1982年   2篇
  1981年   6篇
  1980年   3篇
  1977年   1篇
  1974年   1篇
  1973年   2篇
排序方式: 共有3891条查询结果,搜索用时 937 毫秒
61.
The aim of this work was to investigate, for the first time, the potential of the enzyme glutathione S-transferase I (isoenzyme GST-I) for uses in analytical chemistry. A novel fiber-optic biosensor for the detection and determination of the triazine herbicide atrazine was developed based on maize GST-I expressed in E. coli. The sensing bioactive material was a three-layer mini-sandwich. The enzyme was immobilized on the outer layer that consisted of a hydrophilic polyvinylidenefluoride membrane. This membrane was supported on an inner glass disk by means of an intermediate binder sol–gel layer that incorporated bromcresol green (BCG). The biosensor operated in a static mode at 25 °C and the rate of the enzymatic reaction, using atrazine as a substrate, served as an analytical signal. A calibration curve was obtained for atrazine, with analytically useful concentration range 2.52–125 μM. The sensor detection limit was 0.84 μM. The reproducibility of atrazine sensing was in the order of ±3–5%. The method was successfully applied to the determination of this herbicide in real water samples, without sample preparation steps. Atrazine recovery ranged between 85 and 110%. No interference from other pesticides, such as alachlor and carbaryl was observed in the absence of atrazine. The immobilized enzyme retained about 75% of its original activity after 1 month use. Simply unscrewing the terminal holding ring of the probe and placing a new bioactive sandwich could easily replace a deteriorated mini-sandwich.  相似文献   
62.
The sol–gel method has been used for the synthesis of borosilicate gels from mixtures of methyltriethoxysilane (MTES) and dimethyldiethoxysilane (DMDES) and boric acid. The use of boric acid, B(OH)3 allows the hydrolysis and condensation of hybrid silicon alkoxides without further addition of water or catalyst. The use of difunctional silicon units, –(CH3)2SiO– promote the formation, during the sol–gel process, of linear oligomers which facilitate fiber drawing before gelation. Gel characterization performed by FT-IR, XRD, TG-DTA and DCS analysis indicates the formation of a mixed network with incorporation of the boron units via =B-O-Si≡ bridges. The formation of borosiloxane bonds seems favored by the presence of DMDES. SiBOC glasses were obtained after pyrolysis of the borosilicate gels in argon atmosphere at 1000 °C. TG-DTA study indicates that the ceramic yield decreases by increasing the amount of DMDES. Gel fibers were successfully prepared from convenient partially-aged solutions by hand drawing. Pyrolysis of the obtained gel fibers under argon atmosphere at 1000 °C open the possibility to produce SiBOC homogeneous glass fibers with diameter as low as 10 μm.  相似文献   
63.
应用高分辨率核磁共振仪研究了一系列不同组成的偏氟乙烯和四氟乙烯共聚物。指出,共振核—CF_2—的化学位移不仅受第一、二邻位基团的影响,也受第三邻位的影响。偏氟乙烯和四氟乙烯以无规共聚进行反应,在共聚反应中的链自由基﹏CF_2·或﹏CH_2·容易增长于CH_2=CF_2的CH_2端,而链自由基﹏CH_2·在偏氟乙烯和四氟乙烯共聚反应中的增长倾向于四氟乙烯。  相似文献   
64.
The surface derivatization of poly(p-phenylene terephthalamide) fiber was studied. The obtained surface-derivatized filaments were packed into a fused-silica capillary to evaluate its surface characteristics by using GC. As the stationary phase for GC the surface-derivatized fibers showed higher retention for alkanes and alkylbenzenes than that with the untreated Kevlar fiber. The improvements on the retention power and the peak shape were observed on the benzyl-modified fibrous stationary phase. The derivatized fibrous materials were also evaluated as the extraction medium in fiber-in-tube SPE, and the effect of the surface modification on the extraction power was compared to the parent fiber. The results indicated that the modified fiber possessed a higher extraction power than the untreated fiber. Based on the facts, the successful modification of the fiber surface was estimated.  相似文献   
65.
光谱实验室的建设和管理   总被引:1,自引:0,他引:1  
阐述冶金、铸造等行业用于金属成分分析的直读发射光谱仪实验室的建设和管理。从仪器的调研、选型,实验室选址,基础设施设备的准备,仪器的安装、调试、验收、日常分析,实验室管理等几个方面,分别作了介绍。  相似文献   
66.
The herbaceous crops that may provide fermentable carbohydrates for production of fuels and chemicals also contain 10–20% protein. Protein coproduction with biomass-derived fuels and chemicals has important advantages: (1) food and fuel production can be integrated, and (2) protein is a high-value product that may significantly improve overall process economics. We report the results of an integrated approach to producing protein and fermentable sugars from one herbaceous species, Coastal Bermudagrass (CBG). The ammonia fiber explosion (AFEX) process makes possible over 90% conversion of cellulose and hemicellulose to simple sugars (about 650 mg reducing sugars/g dry CBG) at 5 IU cellulase/g vs < 20% conversion for untreated CBG. The AFEX treatment also improves protein extraction from CBG; over 80% protein recovery is possible from AFEX-treated CBG vs about 30% recovery from untreated CBG.  相似文献   
67.
聚己内酯聚醚嵌段共聚物和共混物的表面性质对其药物释放行为的影响王卫华,贝建中,王智峰,王身国(中国科学院化学研究所北京100080)关键词聚己内酯聚醚嵌段共聚物,共混物,电子能谱,表面性质,药物释放行为聚己内醋(PCL)具有优良的药物通透性和生物相容...  相似文献   
68.
用热聚法固定指示剂的光纤氧气传感器研究   总被引:5,自引:0,他引:5  
姜德生  陈兴  黄俊 《化学学报》2003,61(8):1281-1286
采用热聚法将甲叉双丙烯酰胺(MBBA)聚合并共价交联在硅烷化的玻璃微珠上 ,同时将指示剂Ru(Ⅱ)-邻啡咯啉配合物物理包埋于聚合物中,研制了一种基于 荧光猝灭原理的光纤氧气传感器,采用NaHSO_3-O_2-MnSO_4体系引发MBBA水溶液热 聚合后应,通过确定NaHSO_3,MnSO_4,MBBA和Ru(phen)_3Cl_2的最佳反应浓度以及 玻璃微珠的尺寸,优化了聚合反应条件,改善了指示剂的固定效果,制备了性能较 好的传感器探头,该传感器的检测下限为5×10~(-6)(V/V),响应时间为10s该传感 器连续工作50min,重复性标准偏差为±1%。  相似文献   
69.
The mass resolution of a time-of-flight (TOF) mass spectrometer is directly proportional to its total flight pathlength. Multi-turn or multi-passage ion optical geometries are necessary to obtain fight distances of sufficient length within reasonable size limitations. We have investigated ion optics for a multi-turn TOF mass spectrometer with electrostatic sectors. The concept of 'perfect' focusing conditions is introduced. Furthermore, a new type of multi-turn TOF mass spectrometer, the MULTUM Linear plus, was developed. It consists of four cylindrical electric sectors and 28 electric quadrupole lenses. It has a vacuum chamber 60 x 70 x 20 cm in size. Mass resolution is demonstrated to increase according to the number of ion cycles. A mass resolution of 350 000 (m/z = 28, FWHM) was achieved after 501.5 cycles. The MULTUM Linear plus analyzer is not simple, however; 28 electric quadrupole lenses are used. In order to reduce the number of ion optical parts, an improved multi-turn TOF mass spectrometer, the MULTUM II, consisting of only four toroidal electric sectors, was also developed. The possibility of tandem mass spectrometric applications using multi-turn TOF mass spectrometers is also discussed.  相似文献   
70.
The rheology of the melt hollow fiber spinning process is examined in the thin filament limit. The resulting thin filament equations are also applicable to single-phase and two-phase extensional flows. Using a novel numerical solution procedure, the sensitivity of the fiber spinning equations to material property and process variations is investigated. Fiber geometry is directly controlled by the mass flowrates of the core and clad fluids while the spinline tension is most strongly influenced by clad viscosity. A maximum can occur in the clad stress profile if a core liquid is used and the ratio of core to clad viscosity increases greatly with temperature. Isothermal spinning of high viscosity clad liquids with either a core gas or liquid is unstable for draw ratios greater than 20.2 as found for solid fibers.  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