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51.
Direct In Situ Investigation of Milling Reactions Using Combined X‐ray Diffraction and Raman Spectroscopy
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M. Sc. Lisa Batzdorf Dipl.‐Chem. Franziska Fischer Dipl.‐Chem. Manuel Wilke Dipl.‐Ing. Klaus‐Jürgen Wenzel Dr. Franziska Emmerling 《Angewandte Chemie (International ed. in English)》2015,54(6):1799-1802
The combination of two analytical methods including time‐resolved in situ X‐ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for a detailed analysis of the key mechanisms of milling reactions. To prove the general applicability of our setup, we investigated the mechanochemical synthesis of four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. The reaction mechanism for each model compound could be elucidated. The results clearly show the unique advantage of the combination of XRD and Raman spectroscopy because of the different information content and dynamic range of both individual methods. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structures and thus obtaining reliable data for mechanistic studies. 相似文献
52.
This paper investigates multiple modeling choices for analyzing the rich and complex dynamics of high-speed milling processes.
Various models are introduced to capture the effects of asymmetric structural modes and the influence of nonlinear regeneration
in a discontinuous cutting force model. Stability is determined from the development of a dynamic map for the resulting variational
system. The general case of asymmetric structural elements is investigated with a fixed frame and rotating frame model to
show differences in the predicted unstable regions due to parametric excitation. Analytical and numerical investigations are
confirmed through a series of experimental cutting tests. The principal results are additional unstable regions, hysteresis
in the bifurcation diagrams, and the presence of coexisting periodic and quasiperiodic attractors which is confirmed through
experimentation. 相似文献
53.
Evaluation of grinding methods for pellets preparation aiming at the analysis of plant materials by laser induced breakdown spectrometry 总被引:1,自引:0,他引:1
It has been demonstrated that laser induced breakdown spectrometry (LIBS) can be used as an alternative method for the determination of macro (P, K, Ca, Mg) and micronutrients (B, Fe, Cu, Mn, Zn) in pellets of plant materials. However, information is required regarding the sample preparation for plant analysis by LIBS. In this work, methods involving cryogenic grinding and planetary ball milling were evaluated for leaves comminution before pellets preparation. The particle sizes were associated to chemical sample properties such as fiber and cellulose contents, as well as to pellets porosity and density. The pellets were ablated at 30 different sites by applying 25 laser pulses per site (Nd:YAG@1064 nm, 5 ns, 10 Hz, 25 J cm−2). The plasma emission collected by lenses was directed through an optical fiber towards a high resolution echelle spectrometer equipped with an ICCD. Delay time and integration time gate were fixed at 2.0 and 4.5 μs, respectively. Experiments carried out with pellets of sugarcane, orange tree and soy leaves showed a significant effect of the plant species for choosing the most appropriate grinding conditions. By using ball milling with agate materials, 20 min grinding for orange tree and soy, and 60 min for sugarcane leaves led to particle size distributions generally lower than 75 μm. Cryogenic grinding yielded similar particle size distributions after 10 min for orange tree, 20 min for soy and 30 min for sugarcane leaves. There was up to 50% emission signal enhancement on LIBS measurements for most elements by improving particle size distribution and consequently the pellet porosity. 相似文献
54.
A sequential injection lab-on-valve (SI-LOV) system was used to develop a new methodology for the determination of iron in wine samples exploiting the bead injection (BI) concept for solid phase extraction and spectrophotometric measurement. Nitrilotriacetic Acid (NTA) Superflow resin was used to build the bead column of the flow through sensor. The iron (III) ions were retained by the bead column and react with SCN− producing an intense red colour. The change in absorbance was monitored spectrophotometrically on the optosensor at 480 nm. It was possible to achieve a linear range of 0.09-5.0 mg L−1 of iron, with low sample and reagent consumption; 500 μL of sample, 15 μmol of SCN−, and 9 μmol of H2O2, per assay. The proposed method was successfully applied to the determination of iron in wine, with no previous treatment other than dilution, and to other food samples. 相似文献
55.
56.
We coin a term of milli-free flow electrophoresis (mFFE) to describe mid-scale FFE with flow rates intermediate to macro-FFE and micro-FFE (μFFE). Introduced decades ago, mFFE did not find practical applications. We revive mFFE, as we view it as a viable purification complement to continuous synthesis in capillary reactors with product flow rates of ~5 to 2000 μL/min, too small for macro-FFE but too large for μFFE. The development of the tandem of continuous synthesis/purification will require the production and evaluation of a large number of prototypes of mFFE devices. As the first step, we developed a fast (<24 h) and economical (~$10) method for prototyping mFFE devices using a robotic milling machine. mFFE prototypes are constructed from two machined matching poly(methyl methacrylate) (PMMA) substrates, which are bonded in 10 min using dichloromethane to provide a strong and irreversible seal. Using the developed prototyping technology, we designed and evaluated 25 prototypes of mFFE devices. By optimizing the feed rates and rotational speeds of the drills, the depth of the electrode channels, the dimensions of the entrance and exit reservoirs, the sample flow rate, and the diameter and position of the sample input, we were able to achieve indefinitely long operation of the device with cycles of alternating 15-min electrophoresis and 0.5-min regeneration (bubble removal). The test analytes, rhodamine B and fluorescein, were baseline resolved by mFFE for flow rates ranging from 10 to 600 μL/min. These results prove that our prototyping approach is suitable for the challenging task of multi-parameter optimization of mFFE devices. 相似文献
57.
J. Hakl L. Kerekes S. Mészáros K. Vad P. Gurin M. Kis-Varga I. Uzonyi S. Szabó D. L. Beke 《Czechoslovak Journal of Physics》2002,52(2):151-154
Magnetically frozen partially disordered state was observed in nanocrystalline bulk iron prepared by ball-milling of microcrystalline Fe. Role of nanostructure and oxidized fraction is pointed out. Altough we have found a small constituent which is proportional to 1/T in the ZFC curve, the magnetization scaling with T
3/2 at high fields and the hysteretic behavior in FC-ZFC curves signalizes the presence of frozen ferromagnet at low temperatures. 相似文献
58.
S. M. Cotes A. F. Cabrera L. C. Damonte R. C. Mercader J. Desimoni 《Physica B: Condensed Matter》2002,320(1-4):274-277
BCC, FCC and HCP phases in Fe–13.7 wt% Mn alloys were studied by Mössbauer spectroscopy and X-ray diffraction, after ball milling. The relative amounts of the HCP and FCC phases increase with milling times up to 9 h and decline afterwards. Preliminary AC susceptibility measurements show that the blocking temperatures change for different milling times. 相似文献
59.
K. S. A. Butcher Afifuddin T. L. Tansley N. Brack P. J. Pigram H. Timmers K. E. Prince R. G. Elliman 《Applied Surface Science》2004,230(1-4):18-23
Metallic gallium was observed on the surfaces of GaN commercial samples following argon ion milling. SIMS measurements confirmed that the commercial GaN had approximately 0.02% bulk oxygen present. The SIMS signal was standardized using a specimen of known oxygen content, as determined by elastic recoil detection analysis using 200 MeV heavy ions of 197Au. Despite this 2–5% oxygen was observed by XPS in the bulk of the GaN after the argon ion milling. This oxygen is believed to be from the original surface oxide that re-cycles on the GaN surface during the ion milling. 相似文献
60.