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Non-metallic inclusions and their relation to the J-integral, Ji, phys, at physical crack initiation for different steels and weld metals (1998)

Deimel, P ; Sattler, E

Springer

Journal of materials science 33 (1998), S. 1723-1736

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ISSN: 1573-4803

Source: Springer Online Journal Archives 1860-2000

Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics

Notes: Abstract For two types of steel, the heat-resistant 12% Cr–steel X 20 CrMoV 12 1 and the fine-grained pressure vessel steel 20 MnMoNi 5 5 (A 508 cl.3), a wide range of toughness values in the upper shelf was realized by different sulfur contents and the inclusion of similar weld metals. Additionally, the pressure vessel steel 22 NiMoCr 3 7 (A 508 cl.2) was also investigated. Tensile, fracture mechanics and Charpy V-notch impact tests, as well as detailed microstructural investigations with respect to the size distribution and density of non-metallic inclusions and precipitates, were carried out. In order to ensure ductile behaviour, a test temperature of 150 °C was chosen. The relevance of two quantitative relations available for the calculation of the J-integral, Ji, phys, at physical crack initiation using tensile test data and microstructural parameters, were examined by comparison with the corresponding experimental Ji, phys-values. Only one quantitative relation was able to give good agreement between calculated and experimental Ji, phys-values. This holds not only for the base materials but also for the weld metals. The importance of the size and density of the non-metallic inclusions became quantitatively obvious with the consequence that their size times density is a decisive parameter for toughness. Observations of void initiation, growth and coalescence illustrate the fracture process. © 1998 Chapman & Hall

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1023/A:1004368213567

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Phosphinophosphiniden-Phosphorane tBu2P—P = P(R)tBu2 aus Li(THF)2[η2-(tBu2P)2P] und Alkylhalogeniden (1996)

Bassowa, A. ; Kovacs, I. ; Matern, E. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 931-934

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ISSN: 0044-2313

Keywords: Formation of tBu2P—P = P(R)tBu2 and (tBu2P)2P—R from Li(THF)2[η2-(tBu2P)2P] and alkyl halides ; R = Me, Et, nPr, iPr, nBu, PhCH2, CH2—CH = CH2, CF3 ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: The Phosphinophosphinidene-phosphoranes tBu2P—P = P(R)tBu2 from Li(THF)2[η2-(tBu2P)2P] and Alkyl HalidesWe report the formation of tBu2P—P = P(R)tBu2 a and (tBu2)2PR b (with R = Me, Et, nPr, iPr, nBu, PhCH2, H2C = CH—CH2 and CF3) reactions of Li(THF)2[η2-(tBu2P)2P] 2 with MeCl, MeI, EtCl, EtBr, nPrCl, nPrBr, iPrCl, nBuBr, PhCH2Cl, H2C = CH—CH2Cl or CF3Br. In THF solutions the ylidic compounds a predominate, whereas in pentane the corresponding triphosphanes b are preferrably formed. With ClCH2—CH = CH2 only b is produced; CF3Br however yields both tBu2P—P = P(Br)tBu2 and tBu2P—P = P(CF3)tBu2, but no b. The ratio of a:b is influenced by the reaction temperature, too. The compounds tBu2P—P = P(Et)tBu2 4a and (tBu2P)2PEt 4 b, e. g., are produced in a ratio of 4:3 at -70°C in THF, and 1:1 at 20°C; whereas 1:1 is obtained at -70°C in pentane, and 1:2 at 20°C. Neither tBuCl nor H2C = CHCl react with 2. The compounds a decompose thermally or under UV irradiation forming tBu2PR and the cyclophosphanes (tBu2P)nPn.

Notes: Es wird über die Bildung von tBu2P—P = P · (R)tBu2 a und (tBu2P)2PR b, R = Me, Et, nPr, iPr, nBu, PhCH2, CH2—CH = CH2, CF3 bei Umsetzungen von Li(THF)2 · [η2-(tBu2P)2P] 2 mit MeCl, MeI, EtCl, EtBr, nPrCl, nPrBr, iPrCl, nBuBr, PhCH2Cl, ClCH2—CH = CH2 und CF3Br berichtet.Neben den ylidischen Verbindungen a bilden sich die entsprechenden Triphosphane (tBu2P)2PR b, wobei in THF-Lösung die Bildung von a, in Pentan-Lösung die von b begünstigt ist. Mit ClCH2—CH2 = CH2 bildet sich nur b, mit CF3Br dagegen die Ylide tBu2P—P = P(Br)tBu2 und tBu2P—P=P(CF3)tBu2, aber kein Phosphan b.Das Verhältnis zwischen a und b wird auch durch die Reaktionstemperatur beeinflußt. So bildet 2 mit EtBr in THF bei -70°C die Produkte tBu2P—P = P(Et)tBu2 4a und (tBu2P)2PEt 4 b im Verhältnis 4:3, bei 20°C 1:1; in Pentan bei -70°C 4a:4b = 1:1, bei 20°C 1:2.2reagiert nicht mit tBuCl und H2C = CHCl. Die Verbindungen a zersetzen sich bei UV-Bestrahlung oder beim Erwärmen unter Bildung von tBu2PR und der Cyclophosphane (tBu2P)nPn.

Additional Material: 2 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220603

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Komplexchemie P-reicher Phosphane und Silylphosphane. XII. Bildung und Struktur von Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] und (tBu2P)2P—SiMe3Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)

Kovacs, I. ; Krautscheid, H. ; Matern, E. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 1564-1572

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ISSN: 0044-2313

Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.

Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.

Additional Material: 5 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220920

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Reaktionen von tBu2P—P=P(Br)tBu2 mit Phosphanen. Ein Weg zu unterschiedlich substituierten Phosphinophosphiniden-PhosphoranenProfessor Hans Georg von Schnering zum 65. Geburtstag gewidmet (1996)

Kovacs, I. ; Matern, E. ; Sattler, E. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 1819-1822

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ISSN: 0044-2313

Keywords: Phosphanes ; Phosphinophosphinidene-phosphoranes ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Reactions of tBu2P—P=P(Br)tBu2 with Phosphanes A Route to Variously Substituted Phosphinophosphinidene-phosphoranestBu2P—P=P(Br)tBu2 1 reacts with PR3 [R3 = Et3, tBu3, Ph3, (NMe2)3, (NEt2)3, (NEt2)2Me, Me2SiMe3] according totBu2P—P=P(Br)tBu2 + PR3 → tBu2P—P=PR3 + tBu2PBrWhile 1 decomposes above -30°C yielding tBu2PBr and the cyclophosphanes (tBu2P)3P3 and (tBu2P)4P4, there is no condensation to give any cyclophosphanes from the intermediately formed tBu2P—P in the presence of PR3. The chlorophosphanes tBu2PCl, tBuPPhCl, (Et2N)2PCl and Ph2PCl as well as (CF3)2PBr react quite analogously to the above equation yielding tBu2P—P=P(Cl)tBu2, tBu2P—P=PtBuPhCl, tBu2P—P=P(NEt2)2Cl and tBu2P—P=P(NEt2)2Br.

Notes: tBu2P—P=P(Br)tBu2 1 reagiert mit PR3 [R3 = Et3, tBu3, Ph3, (NMe2)3, (NEt2)3, (NEt2)2Me, Me2SiMe3] nachtBu2P—P=P(Br)tBu2 + PR3 → tBu2P—P=PR3 + tBu2PBrWährend 1 oberhalb -30°C unter Bildung von tBu2PBr und der Cyclophosphane (tBu2P)3P3, (tBu2P)4P4 zerfällt, unterbleibt die Kondensation des intermediär auftretenden tBu2P—P zu den Cyclophosphanen in Anwesenheit von PR3 aufgrund der Addition des Phosphans. Die Chlorphosphane tBu2PCl, tBuPhPCl, (Et2N)2PCl und Ph2PCl sowie (CF3)2PBr reagieren weitgehend entsprechend Gl. (1) unter Bildung von tBu2P—P=PtBu2Cl, tBu2P—P=PtBuPhCl, tBu2P—P=P(NEt2)2Cl, tBu2P—P=P(NEt2)2Br.

Additional Material: 4 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966221104

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