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71.
Jinmao You Xiangming Chen Xianen Zhao Yourui Suo Honglun Wang Yulin Li Jing Sun 《Chromatographia》2006,63(7-8):337-343
A pre-column derivatization method for the sensitive determination of amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl
chloroformate (BCIC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed.
Identification of derivatives is carried out by high performance liquid chromatography/atmospheric pressure chemical ionization
(LC-APCI-MS-MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent is replaced by 1,2-benzo-3,4-dihydrocarbazole-9-isopropyl
functional group, which results in a sensitive fluorescence derivatizing reagent BCIC-Cl. BCIC-Cl can easily and quickly label
amines. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography and show an intense
protonated molecular ion corresponding m/z [MH]+ under APCI in positive-ion mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 260 corresponding to the cleavage of CH2-OCO bond. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0–10.0. Maximal yields close to
100% are observed with a 3 to 4-fold molar reagent excess. In addition, the detection responses for BCIC derivatives are compared
with those obtained using CEOC and FMOC as derivatization reagents. The ratios of IBCIC/ICEOC and IBCIC/IFMOC are, respectively, 1.23–3.14 and 1.25–3.08 for fluorescent (FL) responses (here, I is relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C8 column. Detection limits are calculated from 1.0 pmol injection, at a signal-to-noise ratio of 3, are 10.6–37.8 fmol. The
mean interday accuracy ranges from 94 to 105% for fluorescence detection with the largest mean %CV<7.5. The mean interday
precision for all standards is < 6.0% of the expected concentration. Excellent linear responses are observed with coefficients
of > 0.9997.
Revised: 12 December 2005 and 13 Febrauary 2006 相似文献
72.
A procedure for the Raman spectra calculation of vitreous and molten silicates was presented in this paper. It includes molecular dynamics MD simulation for the generation of equilibrium configurations, Wilson's GF matrix method for the calculations of eigenfrequencies and corresponding vectors, electro-optical parameters method (EOPM) for the Raman intensity calculations, and the bond polarizability model (BPM) for the determination of polarizability and polarizability derivative. One of the most important characteristics of this procedure is the achievement of the partial Raman spectra of five tetrahedral units, as well as the total spectral envelope. In this paper, the calculation was carried out for the vitreous and molten calcium silicates with different compositions and at various temperatures. It is worthwhile to note that the calculation is based on statistical configurations distribution in the space and so it is not needed to artificially adjust the full width at half maximum (FWHM) of spectra. It was also tested through the good agreement of the calculated spectra with the experimental, including some regularity of spectral properties. According to the calculation, the symmetrical stretching of whole tetrahedral units, to which the stretching of Si-O(nb) bond gives the main contribution to intensity, is proven to be the dominance in the high-frequency range (800-1200 cm(-1)) and the symmetrical bending of Si-O(b)-Si, to which the stretching of Si-O(b) bond exhibits the main contribution, is the dominance in the medium-frequency range (400-700 cm(-1)). As the first theoretical results, the Raman scattering coefficient of each Q(i) was found little change along with the variation of composition and temperature. 相似文献
73.
Haoshuang Gu Yongming Hu Hao Wang Xiangrong Yang Zhenglong Hu Ying Yuan Jin You 《Journal of Sol-Gel Science and Technology》2007,42(3):293-297
Single crystalline nanowires of lead titanate (PbTiO3) were fabricated by hydrothermal method at 200°C using lead acetate and n-tetrabutyl titanate as starting materials, where sodium hydroxide was served as a mineralizer. Crystalline phases, microstructure
and optical properties of PbTiO3 nanowires were investigated. The PbTiO3 nanowires were uniform and continuous along the long axis, and were composed of single crystalline PbTiO3 with a tetragonal perovskite structure. The diameter of a single nanowire was around 12 nm and the length reached up to 3 μm.
The chemical composition of the samples and the valence states of elements were determined by X-ray photoelectron spectroscopy
(XPS). The ultraviolet/visible absorption spectroscopic investigation suggested that the absorption edge of optical transition
of the first excitonic state occurred at around 320 nm. A blue-green light emission peaking at about 471 nm (2.63 eV) is observed
at room temperature, and the intensity of this emission increased with increasing excitation wavelength. Oxygen vacancies
are responsible for the light emission of PbTiO3 nanowires. 相似文献
74.
Three ion-pair complexes, [RbzPy](+)[Ni(mnt)(2)](-) (mnt(2)(-) = maleonitriledithiolate; [RbzPy](+) = 4-R-benzylpyridinium; R = Br (1), Cl (2), and NO(2) (3)), with unusual magnetic properties have been synthesized and characterized. The crystal structures of 1 and 2 have been solved. The two complexes belong to the P2(1)/c space group with Z = 4 and C(20)H(11)BrN(5)NiS(4), a = 12.0744(17) A, b = 26.369(4) A, c = 7.440(3) A, and beta = 102.63(3) degrees for 1 and C(20)H(11)ClN(5)NiS(4), a = 12.105(2) A, b = 26.218(4) A, c = 7.374(2) A, and beta = 102.55(2) degrees for 2, respectively. The [Ni(mnt)(2)](-) anions in 1-3 form uniformly spaced one-dimensional (1-D) magnetic chains of s = 1/2 at room temperature. The temperature dependences of the susceptibility for 1-3 show that they undergo phase transitions. All three complexes are paramagnetic in their high-temperature (abbreviation HT) phase and diamagnetic in the low-temperature (abbreviation LT) phase because of strong dimerization along the stacking direction. The results of thermal analysis (DSC) further confirm that the phase transition for 1 and 2 is first-order but maybe second-order for 3. The phenomena observed in this study are similar to those of the 1-D radical systems. 相似文献
75.
JiangBinXIA FuYouLI ShuMingYANG ChunHuiHUANG 《中国化学快报》2004,15(5):619-622
Composite nanoporous electrode SnO2/TiO2 was fabricated for the dye sensitized solar cell (DSSC) with N3 (Cis-Ru). After introducing of TiO2, the open-circuit photovoltage (Voc) was higher than that of the pure SnO2 electrode, while short-circuit photocurrent (Isc) was varied with the ratio of the TiO2. Appropriate content of the TiO2 can be beneficial to the efficiency of the solar cell, and it gives negative impact on the composite electrode when the content of TiO2 is higher. 相似文献
76.
Characterization and electrochemical investigation of boron-doped mesocarbon microbead anode materials for lithium ion batteries 总被引:1,自引:0,他引:1
Mao-Hui Chen Guo-Tao Wu Guang-Ming Zhu Jin-Kua You Zu-Geng Lin 《Journal of Solid State Electrochemistry》2002,6(6):420-427
The structure and anodic performance of boron-doped and undoped mesocarbon microbeads (MCMBs) have been comparatively studied
and the results obtained by XPS, XRD, SEM, Raman spectroscopy and electrochemical measurements are discussed. It is found
that boron doping introduces a depressed d
002 spacing and the larger amount of "unorganized carbon", which induces vacancy formation in the graphite planes and leads to
a quite different morphology from that of the undoped material. Electrochemical charge/discharge cycle tests indicated that
after boron doping the lithium intercalation was carried through at a somewhat higher potential, being attended by greater
irreversible capacity loss.
Electronic Publication 相似文献
77.
Synthesis of a Photolabeling Probe for the Study of Antiviral Mechanism of Ribavirin 总被引:1,自引:0,他引:1
QiongYouwu XunZHU JinQiaoWAN FanQiQU LingPENG 《中国化学快报》2004,15(8):907-910
Ribavirin has been used in urgency to treat SARS patients recently. In order to study its antiviral mechanism by photolabeling approach, we have synthesized and characterized 5-azido-1-β-D-ribofuranosyl-1,2,4-triazole-3-carboxiamide 1 as a photolabeling probe of ribavirin. The azidotriazole nucleoside showed rapid and clean photochemical reaction, suggesting that 1 is a promising probe to study the antiviral mechanism ofribarivin by photolabeling. 相似文献
78.
79.
流动分析法同时测定铬(Ⅵ)及铬(Ⅲ)过程中铈(Ⅳ)氧化剂的影响 总被引:3,自引:0,他引:3
以Ce(Ⅳ)为氧化剂,采用流动分析在线氧化技术,实现了对Cr(Ⅵ)和Cr(Ⅲ)的同时在线分析,发现Ce(Ⅳ)氧化剂在测定过程中产生负干扰,在而Cr(Ⅲ)存在时会使Cr(Ⅵ)的测定结果偏高,本文提出了一个校正模型,通过数学方法消除上述干扰,所建立的分析方法对Cr(Ⅵ)和Cr(Ⅲ)分析的平均相对误差不大于6.5%。 相似文献
80.
镧系元素杂多钼磷酸钾的合成与性质研究 总被引:6,自引:0,他引:6
本文首次报道了K_(17)[Ln(P_2Mo_(17)O_(61))_2]·xH_2O(Ln=La~(3+),Ce~(3+),pr~(3+),Nd~(3+),Sm~(3+),Eu~(3+),Gd~(3+),Tb~(3+),Yb~(3+))的合成方法,取测定结果表明,与(?)系离子配位的配体P_2Mo_(17)O♂♀~-为α_2-型,Ln的配位数为8,推测其结构类似于K_(16)[Ce(Ⅳ)(α_2-P_2W_(17)O_(61))_2]·xH_2O,还进行了UV光谱、CV、极谱、TG-DTA及磁化率等性质的研究。 相似文献