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Flexible ceramic nanofiber preparation method without adding polymer template

A nanofiber technology that does not need to be added. It is applied in the direction of inorganic raw materials such as artificial filaments. It can solve the problems of ceramic nanofibers with many defects, uneven diameters, and low production efficiency. performance, to achieve the effect of continuous production

Pending Publication Date: 2022-03-25
DONGHUA UNIV
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Problems solved by technology

However, the obtained ceramic nanofibers have many defects, uneven diameters, and poor flexibility. In addition, the calcination of polymers also causes defects such as low production efficiency, large production pollution, and high production risks, making it difficult to achieve continuous production.
Some researchers have prepared flexible ceramic nanofiber materials by adjusting the type and amount of organic polymer templates, adjusting the atmosphere and temperature of calcination, but the flexibility of this type of fiber material comes from the aggregate structure, not the fiber material itself, the fiber material itself Easy to break, large grains due to high temperature calcination, still poor in flexibility and strength
Some researchers doped other elements to inhibit the grain growth during fiber ceramicization, but this method introduced heteroatoms and could not obtain pure oxide ceramic nanofibers
Some researchers have adopted different ceramization methods, such as voltage-loaded flash firing process and microwave sintering process, but due to the lack of high-temperature calcination process, there are still a large number of organic components and impurities in ceramic nanofiber products

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  • Flexible ceramic nanofiber preparation method without adding polymer template
  • Flexible ceramic nanofiber preparation method without adding polymer template
  • Flexible ceramic nanofiber preparation method without adding polymer template

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preparation example Construction

[0093] The invention provides a method for preparing flexible ceramic nanofibers without adding a polymer template, which specifically includes the following steps:

[0094] Step 1: Add monodentate ligands, bridging ligands and inorganic precursors into a complex solvent to perform multiple coordination reactions to obtain a homogeneous transparent solution of a bifunctional precursor. The inorganic precursor in the homogeneous transparent solution The body content is 10-50wt%, the monodentate ligand content is 0.1-10wt%, and the bridging ligand content is 0.1-10wt%;

[0095] Step 2: Perform layered and reverse stirring on the obtained homogeneous transparent solution to generate multiple micro-turbulent flows that collide with each other in the solution, so that the materials are evenly collided and dispersed;

[0096] Step 3: Pass cold and humid air into the above layered and reversely stirred solution to promote the hydrolysis-polycondensation reaction of the bifunctional p...

Embodiment 1

[0140] A polymer-free template preparation method for flexible ceramic nanofibers, the specific steps are as follows:

[0141]The first step: add hydrochloric acid, acetylacetone and titanium isopropoxide into the composite solvent of isopropanol and dichloroethane in sequence, and stir at 500rad / min at 30°C for multiple coordination reactions for 12 hours to obtain bifunctional titanium A homogeneous transparent solution of the precursor; wherein, the content of the inorganic precursor is 30wt%, the content of the monodentate ligand is 0.5wt%, the content of the bridging ligand is 2wt%, and isopropanol accounts for 90wt% in the composite solvent. The average number of functional groups of the functional precursor is 2.2.

[0142] Step 2: layered reverse stirring is carried out on the homogeneous transparent solution of the above-mentioned titanium precursor, the rotational speed of the central stirring source is 500 rad / min, and the rotational speed of the reverse stirring so...

Embodiment 2

[0152] A polymer-free template preparation method for flexible ceramic nanofibers, the specific steps are as follows:

[0153] Step 1: Add hydrochloric acid, acetic acid and zirconium isopropoxide in sequence to the composite solvent of isopropanol and N,N-dimethylformamide, and stir at 25°C at 450rad / min for multiple coordination reactions for 10 hours to obtain A homogeneous transparent solution of a bifunctional titanium precursor; wherein, the content of the inorganic precursor is 28wt%, the content of the monodentate ligand is 1wt%, the content of the bridging ligand is 1.5wt%, and the proportion of isopropanol in the composite solvent 92 wt%, the average number of functional groups of the bifunctionality precursor is 2.1.

[0154] Step 2: Perform layered and reverse stirring on the homogeneous transparent solution of the above-mentioned zirconium precursor, the rotational speed of the central stirring source is 400 rad / min, and the rotational speed of the reverse stirrin...

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Abstract

The invention relates to a flexible ceramic nanofiber preparation method without adding a polymer template. The preparation method comprises the following steps: firstly, sequentially adding a monodentate ligand, a bridging ligand and an inorganic precursor into a composite solvent to carry out multiple coordination reaction, then carrying out layered reverse stirring, introducing cold moisture, and carrying out reduced pressure distillation to obtain linear inorganic polymer sol with non-Newtonian fluid characteristics; then carrying out temperature / alkali steam assisted electrostatic spinning on the linear inorganic polymer sol to obtain inorganic gel nanofibers; then introducing the inorganic gel nanofiber into a desorption bath for pressurized desorption, and finally ceramizing the fiber in a pre-burning area and an alternating atmosphere calcining area to obtain the flexible ceramic nanofiber. Compared with the prior art, the method has the advantages that the flexible ceramic nanofibers can be prepared through electrostatic spinning of the linear inorganic sol, the grain size of the flexible ceramic nanofibers is 5-30 nm, the average diameter of the fibers is 50-500 nm, and the softness is smaller than 300 mN.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing flexible ceramic nanofibers without adding polymer templates. Background technique [0002] Ceramic nanofibers are a new class of ceramic materials, which have the advantages of high temperature resistance, corrosion resistance, wear resistance, and good photoelectric performance of ceramic materials, as well as high porosity, large specific surface area, light weight, and small size effect of nanofiber materials. Strong and other characteristics, play a key role in the fields of aerospace, electronic information, clean energy, environmental governance, etc., have extremely high application value, and can generate huge social and economic benefits. At present, ceramic nanofibers are mainly obtained by spinning inorganic sol spinning solution by electrospinning technology. Among them, the properties of inorganic sol and the ceram...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08
CPCD01F9/08C04B35/62259C04B35/6225C04B35/62236C04B2235/656C04B2235/6567
Inventor 丁彬强思雨斯阳刘华磊廖亚龙印霞俞建勇
Owner DONGHUA UNIV