The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)]in a dry nitrogen flow was examined by TG-DTG analysis.The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)]was decomposed into Pr2S3 and deposite...The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)]in a dry nitrogen flow was examined by TG-DTG analysis.The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)]was decomposed into Pr2S3 and deposited carbon in one step where Pr2S3 predominated in the final products.The results of non-isothermal kinetic calculations showed that the decomposition stage was the random nucleation and subsequent growth mechanism(n=2/3),the corresponding apparent activation energy?was 115.89 kJ·mol-1 and the pre-expo-nential constant ln[A/s]was 7.8697.The empirical kinetics model equation was proposed as/(α)=3/2(1-α)[-ln(1-α)]1/3.The X-ray powder diffraction patterns of the thermal decomposition products at 800℃under N2 atmosphere show that the product can be indexed to the cubic Pr2S3 phase.The transmission electron microscopy(TEM)of the final product reveals the particle appearance of a diameter within 40 nm.The experimental results show that the praseodymium sulfide nanocrystal can be prepared from thermal decomposition of Pr[(C5H8NS2)3(C12H8N2)].展开更多
This paper reports two lanthanide complexes of formula (C_9H_7)Ln(C_8H_8)·(THF)_2 where Ln is Pr or Nd,C_9H_7 is indenyl,and C_8H_8 is cyclooctatetraene (COT).The complexes were prepared by the reaction of LnCl_3...This paper reports two lanthanide complexes of formula (C_9H_7)Ln(C_8H_8)·(THF)_2 where Ln is Pr or Nd,C_9H_7 is indenyl,and C_8H_8 is cyclooctatetraene (COT).The complexes were prepared by the reaction of LnCl_3 with K(C_9H_7) and K_2(C_8H_8) in THF.(C_9H_7)Pr(C_8H_8)·(THF)_2 crystallizes in THF at - 15℃ in the monoclinic space group P2_1:with unit cell dimensions a=8.446(0),b=10.083(2), c=13.407(3),β=105.48(1)°,V=1100.43(35)~3,Dc=1.52g/cm^3 and Z=2.The final R value is 0.033,R_w value is 0.030,respectively.In (C_9H_7)Pr(C_8H_8)·(THF)_2 a five-membered ring centroid of C_9H_7,the C_8H_8 ring centroid and the two oxygen atoms from the two THF molecules form a distorted tetrahedral geometry around the metal.展开更多
基金supported by the National Natural Science Foundation of China(Grant No.20171036)Education Committee of Shannxi Province(No.01JK229)
文摘The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)]in a dry nitrogen flow was examined by TG-DTG analysis.The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)]was decomposed into Pr2S3 and deposited carbon in one step where Pr2S3 predominated in the final products.The results of non-isothermal kinetic calculations showed that the decomposition stage was the random nucleation and subsequent growth mechanism(n=2/3),the corresponding apparent activation energy?was 115.89 kJ·mol-1 and the pre-expo-nential constant ln[A/s]was 7.8697.The empirical kinetics model equation was proposed as/(α)=3/2(1-α)[-ln(1-α)]1/3.The X-ray powder diffraction patterns of the thermal decomposition products at 800℃under N2 atmosphere show that the product can be indexed to the cubic Pr2S3 phase.The transmission electron microscopy(TEM)of the final product reveals the particle appearance of a diameter within 40 nm.The experimental results show that the praseodymium sulfide nanocrystal can be prepared from thermal decomposition of Pr[(C5H8NS2)3(C12H8N2)].
文摘This paper reports two lanthanide complexes of formula (C_9H_7)Ln(C_8H_8)·(THF)_2 where Ln is Pr or Nd,C_9H_7 is indenyl,and C_8H_8 is cyclooctatetraene (COT).The complexes were prepared by the reaction of LnCl_3 with K(C_9H_7) and K_2(C_8H_8) in THF.(C_9H_7)Pr(C_8H_8)·(THF)_2 crystallizes in THF at - 15℃ in the monoclinic space group P2_1:with unit cell dimensions a=8.446(0),b=10.083(2), c=13.407(3),β=105.48(1)°,V=1100.43(35)~3,Dc=1.52g/cm^3 and Z=2.The final R value is 0.033,R_w value is 0.030,respectively.In (C_9H_7)Pr(C_8H_8)·(THF)_2 a five-membered ring centroid of C_9H_7,the C_8H_8 ring centroid and the two oxygen atoms from the two THF molecules form a distorted tetrahedral geometry around the metal.
