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Synthesis method of Fe-Si-C ceramic precursor

A technology of ceramic precursor and synthesis method, which is applied in the field of synthesis of precursor highly branched polyferrocenyl silane, can solve the problems of affecting the processing performance of the precursor, solubility reduction, insolubility, etc., and is suitable for large-scale production, The effect of high ceramic productivity and easy operation

Active Publication Date: 2015-04-22
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

H uβler et al. prepared hyperbranched polymers using lithium ferrocene and tetrachlorosilane raw materials, but their solubility Significantly lower (Huβler M., Sun Q., Xu k., et al. Hyperbranched Poly(ferrocenylene)s Containing Groups 14 and 15 Elements: Syntheses, Optical and Thermal Properties, and Pyrolytic Transformations into Nanostructured Magnetoceramics[J]. J. Inorg. Organomet. P., 2005, 15(1): 67-81.), although highly branched PFS has relatively High ceramic yield, but its solubility is significantly reduced or even insoluble, which affects its processing performance as a precursor, and cannot be an ideal precursor of Fe-Si-C ceramics
[0007] In summary, it is difficult for PFS in the prior art to meet the two indicators of high solubility and high ceramic yield at the same time, which seriously hinders the use of PFS as a pioneer Technology popularization of bulk preparation of Fe-Si-C ceramics

Method used

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  • Synthesis method of Fe-Si-C ceramic precursor
  • Synthesis method of Fe-Si-C ceramic precursor
  • Synthesis method of Fe-Si-C ceramic precursor

Examples

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reference example 1

[0040] Reference example 1: the preparation of ferrocene lithium salt:

[0041] Vacuumize the synthesis reaction system, replace high-purity nitrogen to normal pressure, repeat 3 times; add 10 g (53.8 mmol) ferrocene and 70 mL of anhydrous n-hexane solvent into a dry 250 mL reaction bottle, stir; then add 10 mL (66.7 mmol) of tetramethylethylenediamine; after stirring evenly, add 53 mL of n-hexane solution with a molar concentration of n-butyllithium of 2.4 mol / L dropwise, stir, and react for 10 h; filter under reduced pressure, remove the filtrate, Adopt anhydrous n-hexane to wash the orange-red solid filter residue 3 times, and vacuum-dry to remove the n-hexane in the filter residue to obtain 13.3 g ferrocene lithium salt (Fe(η-C 5 h 4 Li 2 )·2 / 3TMEDA). The dried lithium ferrocene salt was stored in an argon-protected glove box.

Embodiment 1

[0043] (1) Vacuumize the synthesis reaction system, replace high-purity nitrogen to normal pressure, repeat 3 times, take 5 g (18.2 mmol) of ferrocene lithium salt prepared in Reference Example 1 in a 250 mL reaction bottle in the glove box, After sealing, remove it and place it in a -20°C reaction bath, inject 50 mL of anhydrous tetrahydrofuran (THF) with a syringe, and stir to obtain component a; (2) Add 0.94 g (7.3 mmol) of Cl 2 Si(CH 3 ) 2 Dissolve in 30 mL of anhydrous THF, add dropwise to component a obtained in step (1) through a constant pressure dropping funnel, and stir at -20°C for 1 h to obtain component b; (3) add 1.09 g (7.3 mmol) Cl 3 Si CH 3 Dissolve in 30 mL of anhydrous THF, add dropwise to component b obtained in step (2) through a constant pressure dropping funnel, and stir for 12 hours at 25°C to obtain component c; (4) in step (3 ) Add 1 mL of methanol dropwise to the obtained component c to terminate the reaction, filter to obtain 110 mL of filtrate,...

Embodiment 2

[0051] (1) Vacuumize the synthesis reaction system, replace high-purity nitrogen to normal pressure, repeat 3 times, take 5 g (18.2 mmol) of ferrocene lithium salt prepared in Reference Example 1 in a 250 mL reaction bottle in the glove box, After sealing it, remove it and place it in a reaction bath at 25°C; inject 100mL of anhydrous n-hexane with a syringe and stir to obtain component a; (2) add 1.1 g (7.7 mmol) of Cl 2 SiCH 3 CH 2 CH 3 Dissolve in 30 mL of anhydrous n-hexane, add dropwise to component a obtained in step (1) through a constant pressure dropping funnel, stir and react for 3 h at 25°C to obtain component b; (3) add 1.2 g (7.3 mmol) Cl 3 Si CH 2 CH 3 Dissolve in 30 mL of anhydrous n-hexane, add dropwise to component b obtained in step (2) through a constant pressure dropping funnel, stir and react at 30°C for 15 hours to obtain component c; (4) in step ( 3) Add 1 drop of deionized water to the obtained component c to terminate the reaction, filter to obta...

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Abstract

The invention relates to a synthesis method of a Fe-Si-C ceramic precursor, which comprises the following steps: (1) vacuumizing the system, replacing with inert gas to normal pressure, taking ferrocene lithium salt, and adding an anhydrous organic solvent to obtain a component a; (2) dissolving a bifunctional halogen-group-containing organosilane compound in an anhydrous organic solvent, and adding the component a to react, thereby obtaining a component b; (3) dissolving a trifunctional halogen-group-containing organosilane compound in an anhydrous organic solvent, and adding the component b to react, thereby obtaining a component c; (4) adding a protonic solvent into the component c to terminate the reaction, filtering, concentrating the filtrate, dropwisely adding the concentrated filtrate into a protonic solvent, filtering, collecting the filter residue, cleaning, and carrying out vacuum drying to obtain the highly-branched polyferrocenyl silane which is the Fe-Si-C ceramic precursor. The Fe-Si-C ceramic precursor prepared by the method has the advantages of controllable molecular composition and structure, high yield, favorable solubility and high ceramic yield, and can be used as an ideal ceramic precursor.

Description

technical field [0001] The invention relates to a synthesis method of a Fe-Si-C ceramic precursor, in particular to a synthesis method of a Fe-Si-C ceramic precursor highly branched polyferrocenyl silane. Background technique [0002] Silicon carbide (SiC) ceramics have excellent properties such as high strength, high modulus, high temperature resistance, oxidation resistance, wear resistance and chemical corrosion resistance, and are widely used in many fields such as aviation, aerospace and weaponry. The introduction of the transition metal Fe makes the obtained Fe-Si-C ceramics not only have the advantages of SiC ceramics, but also have certain electromagnetic properties, and can also have certain catalytic properties under certain conditions, which can be used to prepare high-performance nanoelectronic devices, High-density magnetic recording materials, etc., have broad application prospects. [0003] Yajima et al. in Japan prepared SiC ceramics by pyrolyzing polycarbos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 苟燕子王浩童旋毛腾飞王军谢征芳
Owner NAT UNIV OF DEFENSE TECH
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