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991.
Subhra Basak Soma Sen Sambuddha Banerjee Samiran Mitra Georgina Rosair M.T. Garland Rodriguez 《Polyhedron》2007
Three new dinuclear Zn(II) complexes [Zn(L)(μ1,1-N3)Zn(L)(N3)] · 1.5H2O (1), [Zn(L)(μ1,1-NCO)Zn(L)(NCO)] · 1.5H2O (2) and [Zn(L)(μ1,1-NCS)Zn(L)(NCS)(OH2)] (3) have been synthesized from a potentially tetradentate N2O2-donor Schiff base ligand LH, [LH = (OCH3)(OH)C6H3CHN(CH2)2N(CH3)2], which is the condensation product of o-vanillin and 2-dimethylaminoethylamine. All the three complexes 1, 2 and 3 have been characterized by elemental analysis, IR and 1H NMR spectroscopy, TGA and fluorescence studies. Finally, their structures have been established by the single crystal X-ray diffraction method. Structural studies reveal that in complexes 1, 2 and 3 the two Zn(II) centers are held together by a μ2-phenolato oxygen atom and also by an end-on pseudohalide nitrogen (azide for 1; cyanate for 2; thiocyanate for 3) atom. Among the two deprotonated Schiff base ligands present in each complex, one acts as a tetradentate ligand (N2O2 donor set) while the other acts as a tridentate ligand (N2O donor set), having a non-coordinated methoxy group. All the synthesized complexes display intraligand 1(π–π∗) fluorescence and can potentially serve as photoactive materials. 相似文献
992.
Preparation, Characterization and Reaction Behaviour of Sodium and Potassium Hydridosilylamides R2(H)Si—N(M)R′ (M = Na, K) — Crystal Structure of [(Me3C)2(H)Si—N(K)SiMe3]2 · THF The alkali metal hydridosilylamides R2(H)Si—N(M)R′ 1a‐Na — 1d—Na and 1a‐K — 1d‐K ( a : R = Me, R′ = CMe3; b : R = Me, R′ = SiMe3; c : R = Me, R′ = Si(H)Me2; d : R = CMe3, R′= SiMe3) have been prepared by reaction of the corresponding hydridosilylamines 1a — 1d with alkali metal M (M = Na, K) in presence of styrene or with alkali metal hydrides MH (M = Na, K). With NaNH2 in toluene Me2(H)Si—NHCMe3 ( 1a ) reacted not under metalation but under nucleophilic substitution of the H(Si) atom to give Me2(NaNH)Si—NHCMe3 ( 5 ). In the reaction of Me2(H)Si—NHSiMe3 ( 1b ) with NaNH2 intoluene a mixture of Me2(NaNH)Si—NHSiMe3 and Me2(H)Si—N(Na)SiMe3 ( 1b‐Na ) was obtained. The hydridosilylamides have been characterized spectroscopically. The spectroscopic data of these amides and of the corresponding lithium derivatives are discussed. The 29Si‐NMR‐chemical shifts and the 29Si—1H coupling constants of homologous alkali metal hydridosilylamides R2(H)Si—N(M)R′ (M = Li, Na, K) are depending on the alkali metal. With increasing of the ionic character of the M—N bond M = K > Na > Li the 29Si‐NMR‐signals are shifted upfield and the 29Si—1H coupling constants except for compounds (Me3C)(H)Si—N(M)SiMe3 are decreased. The reaction behaviour of the amides 1a‐Na — 1c‐Na and 1a‐K — 1c‐K was investigated toward chlorotrimethylsilane in tetrahydrofuran (THF) and in n‐pentane. In THF the amides produced just like the analogous lithium amides the corresponding N‐silylation products Me2(H)Si—N(SiMe3)R′ ( 2a — 2c ) in high yields. The reaction of the sodium amides with chlorotrimethylsilane in nonpolar solvent n‐pentane produced from 1a‐Na the cyclodisilazane [Me2Si—NCMe3]2 ( 8a ), from 1b‐Na and 1‐Na mixtures of cyclodisilazane [Me2Si—NR′]2 ( 8b , 8c ) and N‐silylation product 2b , 2c . In contrast to 1b‐Na and 1c‐Na and to the analogous lithium amides the reaction of 1b‐K and 1c‐K with chlorotrimethylsilane afforded the N‐silylation products Me2(H)Si—N(SiMe3)R′ ( 2b , 2c ) in high yields. The amide [(Me3C)2(H)Si—N(K)SiMe3]2·THF ( 9 ) crystallizes in the space group C2/c with Z = 4. The central part of the molecule is a planar four‐membered K2N2 ring. One potassium atom is coordinated by two nitrogen atoms and the other one by two nitrogen atoms and one oxygen atom. Furthermore K···H(Si) and K···CH3 contacts exist in 9 . The K—N distances in the K2N2 ring differ marginally. 相似文献
993.
Three new compounds Ca(HF2)2, Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) were obtained in the system metal(II) fluoride and anhydrous HF (aHF) acidified with excessive PF5. The obtained polymeric solids are slightly soluble in aHF and they crystallize out of their aHF solutions. Ca(HF2)2 was prepared by simply dissolving CaF2 in a neutral aHF. It represents the second known compound with homoleptic HF environment of the central atom besides Ba(H3F4)2. The compounds Ba4F4(HF2)(PF6)3 and Pb2F2(HF2)(PF6) represent two additional examples of the formation of a polymeric zigzag ladder or ribbon composed of metal cation and fluoride anion (MF+)n besides PbF(AsF6), the first isolated compound with such zigzag ladder. The obtained new compounds were characterized by X-ray single crystal diffraction method and partly by Raman spectroscopy. Ba4F4(HF2)(PF6)3 crystallizes in a triclinic space group P1¯ with a=4.5870(2) Å, b=8.8327(3) Å, c=11.2489(3) Å, α=67.758(9)°, β=84.722(12), γ=78.283(12)°, V=413.00(3) Å3 at 200 K, Z=1 and R=0.0588. Pb2F2(HF2)(PF6) at 200 K: space group P1¯, a=4.5722(19) Å, b=4.763(2) Å, c=8.818(4) Å, α=86.967(10)°, β=76.774(10)°, γ=83.230(12)°, V=185.55(14) Å3, Z=1 and R=0.0937. Pb2F2(HF2)(PF6) at 293 K: space group P1¯, a=4.586(2) Å, b=4.781(3) Å, c=8.831(5) Å, α=87.106(13)°, β=76.830(13)°, γ=83.531(11)°, V=187.27(18) Å3, Z=1 and R=0.072. Ca(HF2)2 crystallizes in an orthorhombic Fddd space group with a=5.5709(6) Å, b=10.1111(9) Å, c=10.5945(10) Å, V=596.77(10) Å3 at 200 K, Z=8 and R=0.028. 相似文献
994.
A theoretical and experimental study on all-normal-dispersion Yb-doped mode-locked fiber lasers 下载免费PDF全文
We report on a theoretical and experimental study of an all-normal-dispersion (ANDi) Yb-doped mode-locked fiber laser, in which nonlinear polarization rotation (NPR) is used to realize mode-locking without any dispersion compensation. Based on the coupled nonlinear Schrdinger (CNLS) equation, a model simulating the mode-locked process of an allnormal-dispersion ring fiber laser is developed, which shows that the achievement of stable mode-locking depends on the alignment of the polarization controller (PC) along the fast-polarization axis of the fiber, the birefringence intensity, and the net cavity dispersion. According to the theoretical analysis, stable mode-locked pulses with pulse duration 300 ps and average output power 33.9mW at repetition rate 36MHz are obtained. 相似文献
995.
Nikita M. Podvalnyy Alexander I. Zinin Nelly N. Malysheva Roman A. Kunetskiy 《Journal of carbohydrate chemistry》2013,32(5):213-224
A convenient synthesis and separation of α- and β-anomers of methyl (phenyl 3,5-dideoxy-2-thio-5-trifluoroacetamido-D-glycero-D-galacto-nonulopyranosid)onate (6a and 6b) on a multigram scale was developed. Both α- and β-isomers of 6 were obtained as crystals suitable for safe storage. The β-isomer forms a crystalline solvate with methanol. Fully O-trichloroacetylated and O-trifluoroacetylated N-trifluoroacetyl thiosialosides were synthesized in an efficient manner from the β-tetraol 6b. 相似文献
996.
From literature data presently available, the decomposition temperature and the nature of the decomposition reaction of the ternary compound α-AlFeSi (also designated as αH or τ5) are not clearly identified. Moreover, some uncertainties remain concerning its crystal structure. The crystallographic structure and thermochemical behaviour of the ternary compound α-AlFeSi were meticulously studied. The crystal structure of α-AlFeSi was examined at room temperature from X-ray single crystal intensity data. It presents hexagonal symmetry, space group P63/mmc with unit cell parameters (293 K) a=12.345(2) Å and c=26.210(3) Å (V=3459 Å3). The average chemical formula obtained from refinement is Al7.1Fe2Si. From isothermal reaction-diffusion experiments and Differential Thermal Analysis, the title compound decomposes peritectically upon heating into θ-Fe4Al13(Si), γ-Al3FeSi and a ternary Al-rich liquid. Under atmospheric pressure, the temperature of this reversible transformation has been determined to be 772±12 °C. 相似文献
997.
Hollow nanocubes of spinel Co3O4 with the dimension of 20 nm were successfully prepared via a facile and reproducible solvothermal route. The structure and morphology of Co3O4 nanoboxes were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) techniques. And a possible growth mechanism of Co3O4 nanoboxes were suggested that solid Co3O4 nanocubes nucleate in-situ and grow epitaxially from hexagonal β-Co(OH)2 precursors with the structural matching relationship of [0 0 1] β-Co(OH)2//[1 1 1] Co3O4, and then solid Co3O4 nanocubes gradually hollow and convert to single-crystal nanoboxes owing to Ostwald ripening. 相似文献
998.
Thomas Harmening Constanze M. Fehse Rainer Pöttgen 《Journal of solid state chemistry》2011,184(12):3303-3309
The silicides ScTSi (T=Fe, Co, Ni, Cu, Ru, Rh, Pd, Ir, Pt) were synthesized by arc-melting and characterized by X-ray powder diffraction. The structures of ScCoSi, ScRuSi, ScPdSi, and ScIrSi were refined from single crystal diffractometer data. These silicides crystallize with the TiNiSi type, space group Pnma. No systematic influences of the 45Sc isotropic magnetic shift and nuclear electric quadrupolar coupling parameters on various structural distortion parameters calculated from the crystal structure data can be detected. 45Sc MAS-NMR data suggest systematic trends in the local electronic structure probed by the scandium atoms: both the electric field gradients and the isotropic magnetic shifts relative to a 0.2 M aqueous Sc(NO3)3 solution decrease with increasing valence electron concentration and within each T group the isotropic magnetic shift decreases monotonically with increasing atomic number. The 45Sc nuclear electric quadrupolar coupling constants are generally well reproduced by quantum mechanical electric field gradient calculations using the WIEN2k code. 相似文献
999.
Leonardo C. Ferreira Carlos A. L. Filgueiras Lorenzo C. Visentin Jairo Bordinho Manfredo Hrner 《无机化学与普通化学杂志》2008,634(11):1896-1900
The preparation and characterization of two novel HgCl2 and Hg(SCN)2 complexes with bis[N‐(2‐tert‐butylphenyl)imine]acenaphthene is here described. One‐pot reaction techniques were used, leading to high yields of 75 % and 81 %, respectively. The complexes were characterized by microanalysis, i.r. and 1HNMR spectroscopy, and by single crystal X‐ray diffraction. The structures of the complexes present similar characteristics, the most outstanding being the formation of dimers via intermolecular interaction. Whereas the HgCl2 complex shows a unidimensional network due to strong π–π interactions, its Hg(SCN)2 counterpart displays a supramolecular arrangement resulting from non classical hydrogen bond formation. 相似文献
1000.
Black phosphorus, a promising candidate for lithium battery electrodes, can be prepared by a low-pressure transport reaction route representing the first effective and scalable access to this element modification. Crystal sizes larger than 1 cm were obtained at low-pressure conditions in silica ampoules. X-ray phase analyses, EDX, ICP-MS and optical microscopy were applied to characterize the resulting black phosphorus. The present method drastically improves the traditional preparation ways like mercury catalysis, bismuth-flux or high-pressure techniques and represents an easy, non-toxic, fast and highly efficient method to achieve black phosphorus. In contrast to a previously reported low-pressure route the present transport reaction allows an up-scaling to higher masses of starting materials, a larger black phosphorus yield and faster reaction time under retention of the high product crystallinity. 相似文献