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  • 1
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Chemistry of materials 5 (1993), S. 845-850 
    ISSN: 1520-5002
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    s.l. ; Stafa-Zurich, Switzerland
    Key engineering materials Vol. 132-136 (Apr. 1997), p. 1870-1873 
    ISSN: 1013-9826
    Source: Scientific.Net: Materials Science & Technology / Trans Tech Publications Archiv 1984-2008
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Solid State Ionics 38 (1990), S. 271-273 
    ISSN: 0167-2738
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Physics
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 11 (1997), S. 181-194 
    ISSN: 0268-2605
    Keywords: synthesis ; silazanes ; polymer pyrolysis ; non-oxide ceramics ; Si3N4 ; SiC ; crystallization ; ceramic matrix composites ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The goal of this investigation was to optimize the synthesis of silazane-based polymers for processing fibre-reinforced ceramic matrix composites (CMCs). Liquid oligomeric silazanes were synthesized by ammonolysis of chlorosilanes and characterized spectroscopi- cally (FTIR, NMR) as well as by elemental analysis. The silazanes were obtained in high yield and purity. Different functional groups (system S1: Si - H, Si - CH3, Si - CH=CH2) and different degrees of branching in the Si - N backbone [system S2; Si(NH)3, Si(NH)2] were realized in order to study the properties of the silazanes that are dependent on the molecular structure.For processing ceramics via pyrolysis of pre-ceramic oligomers, molecular weight, rheological behaviour, thermosetting and ceramic yield were investigated systematically and correlated with the molecular structure of the silazanes. Low molecular weights (500-1000 g mol-1) as well as low viscosity values (0.1-20 Pa s) enable processing of the silazanes in the liquid phase without any solvent. Due to the latent reactivity of the functional groups, curing of the polymers via hydrosilylation is achieved.Structural changes and weight loss during polymer curing as well as the organic/inorganic transition were monitored by FTIR spectroscopy and differential thermogravimetric analysis. With increasing temperature (room temperature to 800 °C) the hydrogen content decreases from 7 to 〈 0.5 wt% due to the formation of gaseous molecules (NH3, CH4, H2). High ceramic yields up to 80% were reached by branching the oligomers, thus reducing the amount of volatile precursor fragments.Up to 1300 °C, ceramic materials remained amorphous to X-rays. At higher temperatures (1400-1800 °C) either SiC or SiC/Si3N4 composites were selectively crystallized, depending on the pyrolysis conditions. The utility of the optimized precursors for CMCs has been demonstrated by infiltration of fibre preforms and subsequent pyrolysis. © 1997 by John Wiley & Sons, Ltd.
    Additional Material: 13 Ill.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 0044-2313
    Keywords: Phosphorus nitrides ; nitrido sodalites ; transition metals ; synthesis ; structure ; i.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido-Sodalites. II. Synthesis, Crystal Structure, and Properties of M(6+(y/2)-x)H2x[P12N24]Zy with M = Fe, Co, Ni, Mn; Z = Cl, Br, I; 0 ≤ x ≤ 4; y ≤ 2The nitrido sodalites M(6+(y/2)-x)H2x[P12N24]Zy with M = Fe, Co, Ni, Mn; Z = Cl, Br, I; 0 ≤ x ≤ 4; y ≤ 2 are obtained by the reaction of HPN2 or [PN(NH2)2]3 with the metal halogenide MZ2 (T = 700°C). The compounds are isotypic to Zn(7-x)H2x[P12N24]Cl2. An increase of the ionic radii of the cations or anions results in an expansion of the lattice which is caused by an increase of the P—N—P angle. The influence of the cation is more dominant than that of the anion. By reacting [PN(NH2)2]3 with metal halogenide (MZ2) hydrogen free, X-ray amorphous products are obtained. The formation of the chloride-containing P—N-sodalite in this reaction begins at temperatures below 450°C.
    Notes: Die Nitrido-Sodalithe M(6+(y/2)-x)H2x[P12N24]Zy mit M = Fe, Co, Ni, Mn; Z = Cl, Br, I; 0 ≤ x ≤ 4; y ≤ 2 wurden durch Umsetzung von HPN2 bzw. von [PN(NH2)2]3 mit dem jeweiligen Metallhalogenid MZ2 hergestellt (T = 700°C). Sie sind mit Zn(7-x)H2x[P12N24]Cl2 isotyp. Mit steigendem Ionenradius von Kationen oder Anionen findet man eine Aufweitung des Volumens. Dies ist mit einer Vergrößerung des P—N—P-Winkels verbunden. Der Einfluß der Kationen ist dabei stärker als jener der Anionen. Durch Reaktion von [PN(NH2)2]3 mit dem jeweiligen Metallhalogenid MZ2 werden wasserstofffreie P—N-Sodalithe als röntgenamorphe Pulver erhalten. Bei diesen Reaktionen setzt die Bildung der chlorhaltigen P—N-Sodalithe schon unterhalb von 450°C ein.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 588 (1990), S. 19-25 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Lithium Phosphorus Nitride. Preparation and Refinement of the Crystal Structure of LiPN2Pure lithium phosphorus nitride (LiPN2) has been prepared by solid state reaction of the binary nitrides Li3N and P3N5. X-ray powder diffraction data have been used to refine the crystal structure of LiPN2 by the Rietveld full-profile technique (I42d; a = 457.5(2) pm, c = 711.8(3) pm; 31 reflections observed; scan-range: 20° 〈 2Θ 〈 105°; germanium monochromator, CuKα1; R(wp) = 0.059, R(I, hkl) = 0.061). The atomic arrangement derives from the chalcopyrite type of structure. Phosphorus and nitrogen form a threedimensional net of corner sharing PN4-tetrahedra (P—N 164.5(7) pm, P—N—P 123.6(8)°). Lithium cations occupy positions which are nearly tetrahedrally coordinated by nitrogen (Li—N 209.3(10) pm).
    Notes: Reines Lithium-phosphor(V)-nitrid (LiPN2) wurde durch Festkörperreaktion der binären Nitride Li3N und P3N5 erhalten. Die Kristallstruktur von LiPN2 wurde auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I42d; a = 457,5(2) pm; c = 711,8(3) pm; 31 beob. Reflexe 20° 〈 2Θ 〈 105°; Germanium-Monochromator, CuKα1; R(wp) = 0,059; R(I, hkl) = 0,061). Die Kristallstruktur von LiPN2 leitet sich vom Chalcopyrit-Typ ab. Phosphor und Stickstoff bilden ein dreidimensionales Netz eckenverknüpfter PN4-Tetraeder (P—N 164,5(7) pm; P—N—P 123,6(8)°). Die Lithium-Kationen besetzen die verbleibenden Lücken. Sie sind verzerrt tetraedrisch von jeweils vier Stickstoff-Atomen koordiniert (Li—N 209,3(10) pm).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 121-126 
    ISSN: 0044-2313
    Keywords: Phosphorus nitride imide ; preparation ; crystal structure ; i. r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal Structure, and IR-spectroscopic Investigation of Phosphorus Nitride Imide, HPN2Pure and fine crystalline phosphorus nitride imide (HPN2) is obtained by heterogeneous ammonolysis of P3N5 with gaseous NH3 (T = 580°C, p = 30 bar, 6 d). X-ray powder diffraction data has been used to refine the crystal structure of HPN2 by the Rietveld full-profile technique (I42d; a = 461.82(2) pm, c = 702.04(3) pm; Z = 4; 41 reflections observed, 17° 〈 2Θ 〈 125°, CuKα1, germanium monochromator; R(wp) = 0.072, R(I,hkl) = 0.048). In the solid HPN2 contains a three-dimensional framework of corner-sharing PN4-tetrahedra (P—N: 159.9(4) pm; P—N—P: 130.1(4)°. The hydrogen atoms are covalently bonded to half of the nitrogen atoms. The IR spectrum exhibits six vibrational modes v(N—H): 3224; vas(PNP): 1330, 1223; vas(PNHP): 971, 901: δ(PNP): 531 cm-1).
    Notes: Reines und feinkristallines Phosphor(V)-nitrid-imid (HPN2) wurde durch heterogene Ammonolyse von P3N5 mit gasförmigem NH3 (T = 580°C, p = 30 bar, 6d) dargestellt. Die Kristallstruktur von HPN2 wurde auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I42d, a = 461,82(2) pm, c = 702,04(3) pm; Z = 4; 41 beobachtete Reflexe, 17° 〈 2Θ 〈 125°; Cu—Kα1, Germanium-Monochromator; R(wp) = 0,072; R(I,hkl) = 0,048). Im Festkörper ist HPN2 aus einem dreidimensionalen Netz allseitig eckenverknüpfter PN4-Tetraeder (P—N: 159,9(4) pm; P—N—P: 130,1(4)°) aufgebaut. Die H-Atome sind kovalent an die Hälfte der N-Atome gebunden. Im IR-Spektrum werden sechs Schwingungsbanden (v(N—H): 3224; vas(PNP): 1330, 1223; vas(PNHP): 971, 901; δ(PNP): 531 cm-1) beobachtet.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2014-2019 
    ISSN: 0044-2313
    Keywords: Phosphorus nitrides ; nitrido sodalites ; synthesis ; crystal structure ; i.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido Sodalites. I Synthesis, Crystal Structure, and Properties of Zn7-xH2x [P12N24]Cl2 with 0 ≤ x ≤ 3The nitrido sodalites Zn7-xH2x[P12N24]Cl2 with 0 ≤ x ≤ 3 are obtained by heterogeneous pressure-ammonolysis of P3N5 at presence of ZnCl2 (T = 650°C). These compounds are available too by reaction of ZnCl2, (PNCl2)3, and NH4Cl at 700°C. The crystal structures of four representatives of the above mentioned compounds have been refined by the Rietveld full-profile technique using X-ray powder diffractometer data (I43m, a = 821.61(4) to 824.21(1) pm, Z = 1). In the solid a three-dimensional framework of corner-sharing PN4-tetrahedra occurs (P—N: 163.6 pm, P—N—P: 125.6°, mean values) which is isosteric with the sodalite type of structure. In the center of the β-cages Cl- ions have been found, which are tetrahedrally coordinated by Zn2+ ions. The Zn2+ ions are statistically disordered. According to the phase-width observed (0 ≤ x ≤ 3) the Zn2+ ions may be partially replaced each by two hydrogen atoms which on the other hand are covalently bonded to nitrogen atoms of the P—N framework. The IR-spectra of these compounds show characteristic vibrations.
    Notes: Die Nitrido-Sodalithe Zn7-xH2x[P12N24]Cl2 mit 0 ≤ x ≤ 3 wurden durch heterogene Druckammonolyse von P3N5 in Gegenwart von ZnCl2 (T = 650°C) dargestellt. Die Verbindungen sind auch zugänglich durch Umsetzung von ZnCl2, (PNCl2)3 und NH4Cl bei 700°C. Die Kristallstrukturen von vier ausgewählten Vertretern der obigen Verbindungsreihe wurden auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I43m, a = 821,61(4) bis 824,21(1) pm, Z = 1). Im Festkörper liegt eine dreidimensionale Gerüststruktur allseitig eckenverknüpfter PN4-Tetraeder vor (P—N: 163,6 pm, P—N—P: 125,6°, Mittelwerte), die dem Sodalith-Typ entspricht. Im Zentrum der β-Käfige befinden sich Cl--Ionen, die ihrerseits tetraedrisch durch Zn2+-Ionen umgeben sind. Die Zn2+-Positionen sind statistisch besetzt und gemäß der angegebenen Phasenbreite (0 ≤ x ≤ 3) kann ein Teil der Zn2+-Ionen durch jeweils zwei H-Atome ersetzt werden, die ihrerseits kovalent an Stickstoffatome des P—N-Gerüstes gebunden sind. Im IR-Spektrum der Verbindungen werden charakteristische Schwingungsbanden beobachtet.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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