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   1795篇
  免费   192篇
  国内免费   246篇
化学   1277篇
晶体学   13篇
力学   90篇
综合类   16篇
数学   213篇
物理学   624篇
  2024年   3篇
  2023年   33篇
  2022年   67篇
  2021年   79篇
  2020年   87篇
  2019年   76篇
  2018年   55篇
  2017年   58篇
  2016年   94篇
  2015年   87篇
  2014年   85篇
  2013年   130篇
  2012年   176篇
  2011年   186篇
  2010年   114篇
  2009年   115篇
  2008年   131篇
  2007年   95篇
  2006年   98篇
  2005年   78篇
  2004年   70篇
  2003年   45篇
  2002年   29篇
  2001年   32篇
  2000年   22篇
  1999年   39篇
  1998年   19篇
  1997年   25篇
  1996年   21篇
  1995年   19篇
  1994年   10篇
  1993年   9篇
  1992年   11篇
  1991年   4篇
  1990年   5篇
  1989年   5篇
  1988年   6篇
  1987年   2篇
  1986年   2篇
  1985年   2篇
  1983年   2篇
  1982年   3篇
  1981年   1篇
  1979年   1篇
  1976年   1篇
  1973年   1篇
排序方式: 共有2233条查询结果,搜索用时 15 毫秒
41.
A flow injection method combined with Resonance light scattering detection was developed for the determination of protein concentration in human serum samples. This method is based on the enhanced RLS signals of protein binding with the dye acid chrome blue K. The enhanced RLS intensities at 264 nm, in an acidic aqueous solution, were proportional to the protein concentration over the range of 2.0–40.0 μg·mL−1 for human serum albumin (HSA) and the limit of detection (3σ) is 85 ng·mL−1. This method was successfully applied to the quantification of total proteins in human serum samples. The maximum relative standard deviation is less than 2% and the recovery is between 97 and 103% for the standard addition method. The sample throughput was 60 h−1.  相似文献   
42.
A new rapid, selective and sensitive on-line microwave flow injection-kinetic method was developed for spectrophotometric determination of micro amounts of Ir(III), based on its catalytic effect on the m-acetylchlorophosphonazo (CPA-mA) and KIO(4) reaction in NaOH media. An on-line microwave oven was employed to accelerate the reaction. The reaction was followed spectrophotometrically by measuring the decrease of the absorbance of CPA-mA at 580 nm. The effect of five variables for the determination of Ir(III) was optimized by means of a multilayer artificial neural network using extended delta-bar-delta (EDBD) algorithms. Under the optimum experimental conditions, Ir(III) could be determined in the range 0.060-0.60 micro gZZZ;mL(-1) with detection limit of 0.02 micro gZZZ;mL(-1) and the sampling frequency of 34 h(-1). The proposed method was applied to the determination of micro amounts of Ir(III) in refined ore and secondary alloy with the recoveries from 91.4% to 109%.  相似文献   
43.
金属/氮/碳催化剂(M/N/C,M=Fe、Co等)是最有发展前景的非贵金属电催化剂之一,其性能依赖于催化剂表面的活性物种密度.通过常规的热解含氮前驱物与金属盐的方法制得的催化剂往往存在金属活性物种被包埋而不能有效利用的缺点.考虑到石墨相氮化碳(g-C3N4)富含类吡啶氮和亚纳米孔腔结构,将g-C3N4包覆在高导电性碳纳米笼(hCNC)表面,进而利用表层g-C3N4的配位和限域作用锚定大量Co2+离子,获得的Co/g-C3N4/hCNC复合物经热解后形成了活性位高度暴露、导电性好、孔结构丰富的Co/N/C催化剂.800℃热解得到的最优化催化剂在碱性介质中展现出优异氧还原活性,其起始电位(0.97 V)与商业Pt/C催化剂相当,且抗甲醇干扰性能和稳定性优异.此项研究提供了一种构建具有高度暴露活性位的M/N/C催化剂的有效策略.  相似文献   
44.
DeNOx催化剂FeZSM-5/Raney Fe的制备   总被引:1,自引:0,他引:1  
用原位晶化法合成了FeZSM-5/RFe(RFeRaney Fe)催化剂. 合成液的组成为5Na2O*100SiO2*10TPABr*7 000H2O,pH>11.5. 合成液中不含Al,ZSM-5分子筛的骨架Al只来源于Raney Fe的表面. 此法提高了ZSM-5分子筛中骨架Al的稳定性和分子筛上Fe离子的负载量. FeZSM-5/RFe用作DeNOx催化剂时具有较高的活性和水热稳定性.  相似文献   
45.
含硫有机化合物在竖式石英燃烧管中,于氧气流下经950℃高温燃烧分解,生成的二氧化硫(或三氧化硫)通过含双氧水的石英棉转化管,转化为硫酸。硫酸泵入电解池后,进行酸-碱库仑滴定。本法操作按时间程序控制进行,每次分析时间为15分钟,分析绝对误差为±0.5%对含磷的有机硫化合物及含钠、铁、铜、钼、镍、镧等金属的有机硫化合物,如在样品上复盖一层三氧化钨进行燃烧分解,也可获得满意的结果。  相似文献   
46.
A new solid phase extractant, sinapinaldehyde (SA) modified SBA-15 mesoporous silica, was developed for selective extraction and preconcentration of trace Pb(II) from aqueous solutions. The successful immobilization of SA on SBA-15 and the strong interaction between SA-SBA-15 and Pb(II) were characterized and confirmed by FTIR spectroscopy and scanning electron microscopy. Parameters such as solution pH, shaking time, eluent condition and sample volume were optimized so that the maximum removal of Pb(II) from solution could be achieved. At pH 4.0, the maximum adsorption capacity of the sorbent for Pb(II) was found to be 33.6?mg?g?1 and the adsorbed Pb(II) could be completely eluted using a mixed solution of 2?M HCl and 5% CS(NH2)2. Some common metal ions such as K(I), Na(I), Mg(II), Ca(II), Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) did not interfere with the adsorption of trace Pb(II). The detection limit of the present method was found to be 1.3?ng?mL?1 and the relative standard deviation was less than 2.0% (n?=?8). These results suggested that this new sorbent is very efficient and selective for the removal of trace Pb(II) in water samples.  相似文献   
47.
王建中  黄立军 《应用声学》2017,25(12):153-157
针对目前各行业数字化、智能化产品应用日趋广泛,数据的获取、传输、分析、应用尤为重要,如何避免采集设备接口单一、功能固定、实用性差等缺点,提出采用ARM嵌入式工控模块M9080-N20为基础,采用VK3266串口芯片扩展UART串行接口,提出基于73K222AU调制解调器、HR219307变压器实现采集器二线模拟通信,并支持以太网、CAN总线和UART串行通信,可以有效解决数据远程采集、传输和控制,适用于特殊环境设备故障检测、诊断和抢修。实验结果证明,智能数据采集器不仅具有多种型号设备故障诊断功能;还能实现野外快速通信组网,不同类型设备数据远程采集、传输、分析和控制功能,在军民融合产品上具有广阔的应用前景和实用价值。  相似文献   
48.
49.
A series of novel low band gap polymers containing conjugated side chains with 4,7‐dithien‐5‐yl‐2,1,3‐benzodiathiazole and different electron‐withdrawing end groups of aldehyde ( PT‐DTBTCHO ), 2‐ethylhexyl cyanoacetate ( PT‐DTBTCN ), 1,3‐diethyl‐2‐thiobarbituric acid ( PT‐DTBTDT ), and electron‐donating end group of 2‐methylthiophene ( PT‐DTBTMT ) have been designed and synthesized. All polymers exhibit good solubility in common organic solvents, film‐forming ability, and thermal stability. These conjugated polymers show the broad ultraviolet‐visible absorption and the narrow optical band gaps in the range of 1.65–1.90 eV. Through changing the end group of conjugated side chains, the photophysical properties and energy levels of the polymers were tuned effectively. Bulk heterojunction solar cells based on the blend of these polymers and (6,6)‐phenyl‐C61‐butyric acid methyl ester (PC61BM) reached the best power conversion efficiency (PCE) of 2.72%. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012  相似文献   
50.
In the present work, gold nanocluster (GNC) induced by bovine serum albumin (BSA) was synthesized as a novel fluorescence probe to detect nitrite (NO2 ?) sensitively and selectively. The fluorescence of GNC was found to be quenched effectively by NO2 ?. Under the optimum conditions, it was found that the change of fluorescence intensity was proportional with the concentration of NO2 ? in the linear range of 0.1–50 μM (R?=?0.9990), with a detection limit (S/N?=?3) of 30 nM. The absorption spectroscopy, circular dichroism (CD), and X-ray photoelectron spectroscopy (XPS) studies were employed to discuss the quenching mechanism. In addition, the present approach was successfully applied in real water samples.  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