A kind of flexible pd/sioc nano fiber mat and preparation method thereof

A nanofiber and flexible technology, applied in the field of flexible Pd/SiOC nanofiber felt and its preparation, can solve the problems that the mechanical strength and flexibility of the silica nanofiber felt cannot meet the requirements of high temperature filtration and nanocomposite materials, and can achieve a wide range of applications. The effect of citing prospects, good flexibility, and improving mechanical properties

Active Publication Date: 2019-05-10
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a flexible Pd / SiOC nanofiber mat and its preparation method, which solves the problem that the mechanical strength and flexibility of the silica nanofiber mat obtained in the prior art cannot meet the requirements in the field of high-temperature filtration and nanocomposite materials technical problem

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  • A kind of flexible pd/sioc nano fiber mat and preparation method thereof
  • A kind of flexible pd/sioc nano fiber mat and preparation method thereof
  • A kind of flexible pd/sioc nano fiber mat and preparation method thereof

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preparation example Construction

[0029] The preparation method of the flexible Pd / SiOC nanofiber mat provided by the present invention comprises the following steps: the spinning solution is sequentially subjected to electrospinning, pre-oxidation and pyrolysis to obtain a flexible Pd / SiOC nanofiber mat; the spinning solution is made of polystyrene , polycarbosilane, palladium acetylacetonate, xylene and dimethylformamide are mixed in a mass ratio of 3:8-20:0.2-2:30-50:50-70.

[0030] Configure the resulting spinning solution in this way to produce a Pd / SiOC nanofiber mat with higher flexibility. For its flexibility, see figure 1 , it can be seen from the figure that the fiber mat can be well wrapped on the glass surface without breaking. Mixing in this ratio is also beneficial to obtain fibers with uniform diameters after the subsequent electrospinning step. The SEM figure of gained fiber mat sees figure 2 , it can be seen that the fibers contained in the obtained fiber mat have a relatively uniform diame...

Embodiment 1

[0051] (1) Preparation of spinning solution: polystyrene (molecular weight 2,000,000), polycarbosilane (molecular weight 3500), palladium acetylacetonate, xylene and dimethylformamide are added in a mass ratio of 3:8:0.2:30:70 Mix in a reactor, then magnetically stir for 16 hours at a rotating speed of 800 rpm, and stir evenly to obtain a spinning solution;

[0052] (2) Electrospinning: use a metal needle with an inner diameter of 0.8 mm as the nozzle, the spinning voltage is 11 kV, the vertical distance from the needle tip to the receiving screen is 20 cm, the feeding rate is 12 μL / min, the spinning temperature is 20 °C, and the air The relative humidity is 30RH%. Using a drum to collect the filaments, the spinning solution obtained in step (1) is subjected to electrospinning, and the fibril felt is collected;

[0053] (3) Pre-oxidation: Put the fibril mat obtained in step (2) in a programmable temperature-controlled pre-oxidation furnace, and raise the temperature to 200°C ...

Embodiment 2

[0057] (1) Preparation of spinning solution: Add polystyrene (molecular weight 1,200,000), polycarbosilane (molecular weight 3000), palladium acetylacetonate, xylene and dimethylformamide in a ratio of 3:10:0.5:50:50 Mix in a reactor, then magnetically stir for 10 hours at a rotating speed of 600 rpm, and stir evenly to obtain a spinning solution;

[0058] (2) Electrospinning: a metal needle with an inner diameter of 1.5 mm was used as the nozzle, the spinning voltage was 16 kV, the vertical distance from the needle tip to the receiving screen was 25 cm, the feeding rate was 30 μL / min, the spinning temperature was 35 °C, and the air The relative humidity is 40RH%. Using a drum to collect the filaments, the spinning solution obtained in step (1) is subjected to electrospinning, and the fibril felt is collected;

[0059] (3) Pre-oxidation: put the fibril mat obtained in step (2) in a programmable temperature-controlled pre-oxidation furnace, and raise the temperature to 250° C....

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Abstract

The invention provides flexible Pd / SiOC nanofiber felt and a preparation method thereof. The flexible Pd / SiOC nanofiber felt comprises a step (1) of preparing a spinning : mixing polystyrene, polycarbosilane, palladium acetylacetonate, xylene and dimethylformamide, performing magnetic stirring, and obtaining the spinning solution; a step (2) of performing electrostatic spinning; a step (3) of performing preoxidation: performing preoxidation in the air atmosphere; a step (4) of performing pyrolysis: pyrolyzing the pre-oxidized nanofiber felt in the inert atmosphere, and obtaining final flexible Pd / SiOC nanofiber felt. The obtained flexible Pd / SiOC nanofiber is uniform in diameter distribution, has a diameter of 400-550 nm, is composed of nanofiber, has excellent flexibility and high strength, is simple in preparation method, and has wide application prospect.

Description

technical field [0001] The invention relates to the technical field of ceramic fiber mats, in particular to a flexible Pd / SiOC nanofiber mat and a preparation method thereof. Background technique [0002] Ceramic nanofibers have excellent corrosion resistance and oxidation resistance, and can be used as filter materials and catalyst supports in harsh environments. Among the methods for preparing ceramic nanofibers, the electrospinning method combined with the precursor conversion method has attracted much attention because of its simple process and large-scale production. The mechanical properties of nano-oxide or carbide ceramic fibers reported so far are relatively poor, which is related to the low ceramic yield of the precursors used. Precursors with high ceramic yields are beneficial to improve the mechanical properties of the final pyrolyzed ceramic fibers. SiOC ceramics have good high temperature stability and creep properties, and have application prospects in lithi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D04H1/728D04H1/4209D01D5/00
CPCD01D5/003D01D5/0069D01D5/0092D04H1/4209D04H1/728
Inventor 王应德吴楠
Owner NAT UNIV OF DEFENSE TECH
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