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A kind of method for preparing Si-C-O ceramic fiber by conversion of organosilicon resin

A technology of ceramic fiber and silicone, which is applied in the direction of fiber chemical characteristics, textiles and papermaking, single-component synthetic polymer rayon, etc., can solve the problems of large number of holes, no use performance, poor mechanical properties, etc., and achieve mechanical properties Good, low production cost, easy to achieve effect

Active Publication Date: 2020-04-21
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Commonly used methods in the prior art for preparing Si-C-O fibers include: 1) Utilize the conversion of phenyl and propyl silicone resins to prepare ceramic fibers and composite materials. Mixing, the precursor is melt-spun to obtain silicone resin fibrils, and the Si-C-O fiber is prepared by using the non-melting process of ultraviolet radiation + thermal crosslinking. There is obvious two-phase separation in the internal structure of the fiber, resulting in a loose fiber structure and basically no Performance
2) Using the YR3370 silicone resin produced by Momentive Corporation of Japan as a precursor, the fibrils were prepared by melt spinning, and Si-C-O fibers with low carbon content were prepared by atmosphere non-melting, and the non-melting and fiber properties of the fibers were studied under different atmospheres. Oxidation resistance, because the prepared fibers contain more holes and defects, and the carbon content is low, resulting in Si-C-O fibers mainly composed of SiO 2 Composed of free carbon and poor mechanical properties
[0004] Silicone resin is now used to prepare Si-C-O ceramic fibers. The obtained fiber filaments have a large amount of pores, or there is obvious two-phase separation, or the carbon content is low, resulting in poor mechanical properties of the fibers, which are far from meeting the requirements of Si. -C-O ceramic fiber requirements

Method used

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  • A kind of method for preparing Si-C-O ceramic fiber by conversion of organosilicon resin
  • A kind of method for preparing Si-C-O ceramic fiber by conversion of organosilicon resin
  • A kind of method for preparing Si-C-O ceramic fiber by conversion of organosilicon resin

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Embodiment 1

[0032] Prepare Si-C-O ceramic fiber, the present embodiment comprises the following steps:

[0033] (1) Put 10g of solid silicone resin SR8803 in the spinning cylinder of the melt spinning device, pass high-purity nitrogen gas, replace the air at 60°C, heat to 150°C, keep it warm for 0.5h, and under 0.4MPa pressure, at 600r / min of spinning speed for melt spinning to obtain silicone resin fibrils;

[0034] (2) Place the silicone resin fibrils in an ultraviolet cross-linking instrument with an emission wavelength of 254nm, and irradiate for 20 hours to obtain silicone resin infusible fibers;

[0035] (3) Put the non-melting fiber in the graphite furnace, vacuumize, pass high-purity nitrogen to replace the air three times, raise the temperature to 1000°C at a heating rate of 50°C / h, and keep it at this temperature for 1h to obtain Si -C-O ceramic fiber.

[0036] Result analysis:

[0037] figure 1 It is the infrared spectrum of the silicone resin precursor. It can be seen fro...

Embodiment 2

[0041] Prepare Si-C-O ceramic fiber, the present embodiment comprises the following steps:

[0042] (1) Put 10g of solid silicone resin YR3370 in the spinning tube of the melt spinning device, pass high-purity nitrogen into it, replace the air at 60°C, heat to 180°C, keep it warm for 2h, under 0.3MPa pressure, at 600r / The spinning speed of min is melt-spun to obtain silicone resin fibrils;

[0043] (2) Place the silicone resin fibrils in an ultraviolet cross-linking instrument with an emission wavelength of 200nm, and irradiate for 5 hours to obtain silicone resin infusible fibers;

[0044] (3) Put the non-melting fiber in the graphite furnace, vacuumize, pass high-purity nitrogen to replace the air three times, raise the temperature to 900°C at a heating rate of 60°C / h, and keep it at this temperature for 2h to obtain Si -C-O ceramic fiber.

Embodiment 3

[0046] Prepare Si-C-O ceramic fiber, the present embodiment comprises the following steps:

[0047] (1) Put 10g of solid silicone resin SR8803 in the spinning tube of the melt spinning device, pass high-purity nitrogen gas, replace the air at 60°C, heat to 200°C, keep it for 1h, and under the pressure of 0.1MPa, at 300r / / The spinning speed of min is melt-spun to obtain silicone resin fibrils;

[0048] (2) Silicone resin fibrils are placed in a quartz tube furnace, vacuumized, and high-purity nitrogen is introduced to replace the air three times, and an active atmosphere is introduced. The volume of high-purity nitrogen in the active atmosphere is 3 times that of boron trichloride gas, Obtain silicone resin non-melting fiber;

[0049] (3) Put the non-melting fiber in the graphite furnace, vacuumize, pass high-purity nitrogen to replace the air three times, heat up to 1300°C at a heating rate of 80°C / h, and keep it at this temperature for 1h to obtain Si -C-O ceramic fiber. ...

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Abstract

The invention provides a method for converting organic silicon resin to prepare a Si-C-O ceramic fiber. The non-melting of a silicon resin fibril is completed by adopting ultraviolet radiation cross-linking or reactive atmosphere cross-linking; afterwards, the Si-C-O ceramic fiber is prepared through high-temperature sintering. The ultraviolet radiation is used for realizing the cross-linking process of the fibril through enabling the molecule of the organic silicon resin to generate a free radical; a reactive atmosphere is used for realizing cross-linking through reacting with Si-OH; thus, the non-melting process of the fiber is completed; a non-melting and further insoluble three-dimensional network structure is formed; the fibril is enabled to be incapable of generating melting and doubling in a subsequent high-temperature pyrolysis process. The method can be used for reducing the production cost of the Si-C-O ceramic fiber, and the obtained Si-C-O ceramic fiber is enabled to have better mechanical performance.

Description

technical field [0001] The invention belongs to the field of precursor conversion ceramics, and in particular relates to a method for preparing Si-C-O ceramic fibers by conversion of organic silicon resin. Background technique [0002] SiC fiber has excellent high temperature resistance and mechanical properties, and has good compatibility with metals, ceramics, and polymers. It is an ideal inorganic reinforcing fiber and has broad applications in high-tech fields such as aerospace, weaponry, and nuclear industry. However, the high price of SiC fiber is one of the most important reasons that limit the further expansion of its application field. Oxygen-containing SiC fiber, that is, Si-C-O fiber, has good performance at 1200 ° C. Compared with oxide fiber, it has better temperature resistance and acid and alkali corrosion resistance. Compared with SiC fiber, it has the advantage of low preparation cost. , has received more and more attention from researchers in recent years....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/56C04B35/622D01F6/76
CPCC04B35/56C04B35/62277D01F6/76
Inventor 苟燕子李浩王浩简科邵长伟王小宙王兵
Owner NAT UNIV OF DEFENSE TECH
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