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971.
色谱柱分类数据库用于指导天然药物化学对照品色谱纯度测定时色谱柱理性选择 总被引:2,自引:0,他引:2
由于中药化学对照品多数来源于动植物药材,很容易混有结构类似物,故有机杂质测定是可能影响其化学对照品赋值准确性的关键风险因素。中药化学对照品的有机杂质测定通常采用药典收载或文献报道的高效液相色谱法,这些方法通常仅规定“以十八烷基硅烷键合硅胶为填充剂”,无适宜色谱柱的品牌信息,或者实验室无文献所用的色谱柱品牌,而目前市场上已有800多种品牌的C18柱,生产工艺的不同导致不同品牌C18柱的选择性有差异,甚至差异显著。这很容易出现由于色谱柱选择不适宜而导致测定结果不准确的风险。该文采用国外色谱柱分类数据库指导对照品纯度考察时色谱柱的理性选择,尽可能减少色谱柱盲选可能导致的纯度结果不准确的风险。首先,用数据库挑选2根选择性差异显著的色谱柱(选择性因子F≥6)进行平行实验,以尽可能反映采用不同品牌色谱柱可能出现的分离效果差异。如果这2根色谱柱的分离效果及纯度测定结果无显著性差异,则可以交叉验证该对照品纯度测定的准确性。否则需要从数据库中选择另外1根与之前试验中分离效果更好、选择性相似的色谱柱进行纯度结果验证。在N-反式-p-对香豆酰基酪胺和表儿茶素没食子酸酯首批对照品的纯度考察中,使用了上述策略并验证了其有效性和科学性,计划推广应用至更多的中药化学对照品,特别当其可能含碱性或弱酸性化合物时,更应该尝试采用本文推荐的色谱柱选择策略交叉验证其纯度测定结果的准确性。 相似文献
972.
X. F. Yu L. Lu Y. R. Zhong W. G. Luo A J. Wang 《Russian Journal of Coordination Chemistry》2017,43(4):244-251
Three new complexes, namely {[Ln(L)3(2,2′-Bipy)] n · H2O} (Ln = Pr (I), Sm (II), and Nd (III)) (HL = 3-(2-hydroxyphenyl)propanoic acid), have been synthesized and structurally characterized. The structural determinations indicated (CIF files CCDC nos. 1472729 (I), 1472730 (II), 1472734 (III)) that I–III have similar dinuclear structures, which can be further linked into 2D sheet via the hydrogen bond interactions. Furthermore, the luminescent properties of I–III show the strong emissive power and feature. 相似文献
973.
In this paper, we propose a Bayesian semiparametric mean-covariance regression model with known covariance structures. A mixture model is used to describe the potential non-normal distribution of the regression errors. Moreover, an empirical likelihood adjusted mixture of Dirichlet process model is constructed to produce distributions with given mean and variance constraints. We illustrate through simulation studies that the proposed method provides better estimations in some non-normal cases. We also demonstrate the implementation of our method by analyzing the data set from a sleep deprivation study. 相似文献
974.
Ju-Lan Zeng Lei Zhou Yue-Fei Zhang Sai-Ling Sun Yu-Hang Chen Li Shu Lin-Ping Yu Ling Zhu Liu-Bin Song Zhong Cao 《Journal of Thermal Analysis and Calorimetry》2017,129(3):1291-1299
Nine nucleating agents, calcium pimelate (CaPi), bicyclic [1, 2, 2]heptane di-carboxylate (HPN-68), a commercially obtained aryl amide nucleating agent (TMB-5), calcium salt of hexahydrophthalic acid (HPN-20E), 1,3:2,4-di-p-methylbenzylidene sorbitol (MDBS) and sodium, potassium, magnesium and calcium salt of benzene-1, 3, 5-tricarboxylic acid (Na3BTC, K3BTC, Mg3BTC2 and Ca3BTC2, respectively), were applied to reduce the supercooling of erythritol, and their effects were investigated by cyclic differential scanning calorimetry (DSC). The results revealed that Na3BTC and K3BTC could not induce erythritol to crystallize under the experiment condition. MDBS could only make erythritol to crystallize at a temperature slightly higher than that of pure erythritol, and the effect was unstable. Mg3BTC2, Ca3BTC2 and HPN-68 could induce erythritol to crystallize at relatively high temperature, but the peak temperature of crystallizing (T p, cr) and the phase change enthalpy of crystallizing (Δcr H) decreased greatly as the melting–crystallizing cycles increased. HPN-20E-doped erythritol crystallized at a high temperature with the T p, cr of 69.3 °C at the first cycle, but the T p, cr and Δcr H varied greatly during the melting–crystallizing cycles. CaPi and TMB-5 could induce erythritol to crystallize at a stable temperature with the T p, cr of about 69 °C and 64 °C, respectively, and with a stable Δcr H of about 204 and 185 J g?1, respectively, in all melting–crystallizing cycles. Hence, CaPi- and TMB-5-doped erythritol could be used as PCMs and applied in thermal energy storage in which the energy was absorbed at a high temperature and released at a lower but stable temperature. 相似文献
975.
Sai-Bo Yu Ju-Lan Zeng Sai-Ling Sun Lei Zhou Yu-Hang Chen Liu-Bin Song Zhong Cao Li-Xian Sun 《Journal of Thermal Analysis and Calorimetry》2017,129(1):189-199
Solar absorption cooling is a wonderful method to provide cold energy by exploiting solar energy. Phase change materials (PCMs) that store latent thermal energy are indispensible in solar absorption cooling system. It is worthwhile to find new PCMs due to the demanding on the temperature of the stored thermal energy which in turn would power the absorption chiller. In this paper, two compounds: 1-bromo-2-methoxynaphthalene (compound 1) and 2,2′-diphenyl-4,4′-bi(1,3-dioxane)-5,5′-diol (compound 2), were selected as potential PCMs. Their thermal energy storage properties and thermal stability were characterized by differential scanning calorimetry and thermogravimetric analysis. The results showed that both compounds could be applied as good PCMs in solar absorption cooling systems. Compound 1 melted at 356.82 K with the ΔH of 98.81 J g?1, while compound 2 melted in a broad temperature range with the melting point of 466.26 K and the ΔH of 101.4 J g?1. Both compounds exhibited good thermal stability. Furthermore, the molar specific heat capacities of these two compounds were measured by temperature-modulated differential scanning calorimetry from 198.15 K to the temperature that they started to decompose, and the thermodynamic functions of [H T–H 298.15] and [S T–S 298.15] were calculated based on the specific heat capacities data. 相似文献
976.
Jingwei Wang Qianqian Luo Chunhua Luo Hechun Lin Ruijuan Qi Ni Zhong Hui Peng 《Journal of Solid State Electrochemistry》2017,21(7):2071-2077
In this study, MoS2 nanosheets were first prepared by exfoliating its bulk material in HCl/LiNO3 solution with a yield of 45%, and then a facile strategy was developed to synthesize polyaniline/MoS2 (PANI/MoS2) nanocomposite via in situ polymerization. Structural and morphological characterizations of MoS2 nanosheets and the nanocomposite were investigated by scanning electron microscope (SEM), transmission electron microscope (TEM), and X-ray powder diffraction. The results of SEM illustrated that orderly sawtooth polyaniline (PANI) nanoarrays were formed on the surface of MoS2 nanosheets. The nanocomposite displayed good electrochemical performance as a supercapacitor electrode material. The specific capacitance reached 560 F/g at a current density of 1.0 A g?1 in 1.0 M H2SO4 solution. Such good performance is because that the MoS2 nanosheets provided a highly electrolytic accessible surface area for redox-active PANI and a direct path for electrons. 相似文献
977.
Dr. Tian Qin Dr. Lara R. Malins Jacob T. Edwards Rohan R. Merchant Alexander J. E. Novak Jacob Z. Zhong Riley B. Mills Ming Yan Dr. Changxia Yuan Dr. Martin D. Eastgate Prof. Phil S. Baran 《Angewandte Chemie (International ed. in English)》2017,56(1):260-265
Two named reactions of fundamental importance and paramount utility in organic synthesis have been reinvestigated, the Barton decarboxylation and Giese radical conjugate addition. N ‐hydroxyphthalimide (NHPI) based redox‐active esters were found to be convenient starting materials for simple, thermal, Ni‐catalyzed radical formation and subsequent trapping with either a hydrogen atom source (PhSiH3) or an electron‐deficient olefin. These reactions feature operational simplicity, inexpensive reagents, and enhanced scope as evidenced by examples in the realm of peptide chemistry. 相似文献
978.
In this paper, we define a new constrained multi-component KP(cMKP) hierarchy which contains the constrained KP(cKP) hierarchy as a special case. We derive the recursion operator of the constrained multi-component KP hierarchy. As a special example, we also give the recursion operator of the constrained two-component KP hierarchy. 相似文献
979.
A singular integral equation arising in a cruciform crack problem is investigated in the present paper. Based on the convex technique, the piecewise Taylor-series expansion method is extended by introducing a weight parameter. An approximate solution of the singular integral equation is constructed and its convergence and error estimate are made. The variations of the approximate solutions associating with stress intensity factors are analyzed by considering internal pressures of power and sine functions, respectively. By comparing with the known methods, the observations reveal that a good approximation can be achieved using less derivative times, less discretization points, and a suitable weight parameter. The obtained results show that the crack growth is dependent on applied mechanical loadings. 相似文献
980.
Two homoclinic solutions for a nonperiodic fourth‐order differential equation without coercive condition 下载免费PDF全文
In this paper, we investigate the existence of homoclinic solutions for a class of fourth‐order nonautonomous differential equations where w is a constant, and . By using variational methods and the mountain pass theorem, some new results on the existence of homoclinic solutions are obtained under some suitable assumptions. The interesting is that a(x) and f(x,u) are nonperiodic in x,a does not fulfil the coercive condition, and f does not satisfy the well‐known (AR)‐condition. Furthermore, the main result partly answers the open problem proposed by Zhang and Yuan in the paper titled with Homoclinic solutions for a nonperiodic fourth‐order differential equations without coercive conditions (see Appl. Math. Comput. 2015; 250:280–286). Copyright © 2016 John Wiley & Sons, Ltd. 相似文献