Preparation method of Si-Zr-O-C-based ceramic fiber material, product and application

A ceramic fiber and product technology, applied in the field of ceramic fiber material preparation technology, can solve the problems of heat insulation performance and mechanical performance reduction, and achieve the effects of reducing thermal conductivity, enhancing infrared shielding effect, and increasing barrier effect

Pending Publication Date: 2022-01-07

WUHAN TEXTILE UNIV

4 Cites 1 Cited by

AI-Extracted Technical Summary

Problems solved by technology

These ceramic fibers have good thermal insulation or mechanical properties at room temperature, but thei...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Method used

[0065] The phases in the ceramic fiber material obtained in the present invention include ZrO2 phase and SiC phase. Among them, the ZrO2 phase has very low solid thermal conductivity, but poor infrared shielding ability at high temperature, while the SiC phase has high solid thermal conductivity, but excellent high temperature infrared shielding ability. Therefore, the present invention combine...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Abstract

A preparation method of a Si-Zr-O-C-based ceramic fiber material comprises the following steps of: dissolving a zirconium source in a complexing agent to obtain a primary solution; mixing the primary solution, a silicon source and a spinning auxiliary solution to obtain a precursor sol spinning solution; carrying out electrostatic spinning on the precursor sol spinning solution to obtain precursor gel fibers; and sequentially drying and sintering the precursor gel fibers to obtain a final product, namely the ceramic fiber material. The ceramic fiber material can be applied to the field of heat insulation. According to the design, good heat insulation performance and mechanical performance can be both achieved in a high-temperature using environment, the production cost is low, the fiber continuity is good, and the energy consumption is low.

Application Domain

Artifical filament manufacture

Technology Topic

ElectrospinningFiber +2

Image

Examples

Experimental program(7)

Example Embodiment

[0039] See figure 1 and figure 2 A method of preparing Si-Zr-O-C based ceramic fiber material, comprising the steps of:

[0040] Prepared spinning solution taken precursor sol: complexing agent to give a solution, then a solution of the silicon source, the spinning solution was mixed with additives to give a first precursor sol of zirconium source was dissolved in the spinning dope; the said spinning solution additives, auxiliaries solvents, catalysts, additives composed of a solute, said solute aid is any one or any mix of the following: polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl butyral, polyvinyl two alcohol, polyoxyethylene alcohol;

[0041] Precursor gel fibers Preparation: spinning liquid of the sol precursor electrostatic spinning to obtain a precursor gel fibers;

[0042]Ceramic fiber material acquisition: The above precursor gel fibers were sequentially dried, sintered to obtain the ceramic fiber material.

[0043] In the preparation of the precursor sol spun liquid, the zirconium source, the silicon source is hydrolyzed and polycondensation reaction under the action of the auxiliary solvent and the catalyst.

[0044] The zirconium source, a complexing agent, auxiliary solvent, catalyst, and silicon source are any combination of the following:

[0045] Zirconium source: swirtate, quadr propoxy zirconium, n-propanol zirconium, isopropathy, zirconium zirconium zirconium zirconium zirconium zirconium or any mixing;

[0046] Complexing agent: any one or any mixing of citric acid, acetic acid, and acetic acid;

[0047] Auxiliary solvent: any one or any mixing of ethanol, isopropanol, dimethylformamide;

[0048] Catalyst: any one or any mixing of nitric acid, hydrochloric acid, boric acid;

[0049] Silicon source: Ethyl orthosilatate, vinyl trimethoxysilane, methyl triethoxysilane, dimethyl diethoxysilane, polymethylphenylsiloxane in any one or any mixing.

[0050] In the precursor sol spun liquid, the spinning auxiliary solution is from 5 to 10 wt.%.

[0051] The spinning auxiliary solution is from 7.5 wt.%

[0052] The ratio ratio between the zirconium source, a complexing agent, a silicon source, auxiliary solvent, and a catalyst is:

[0053] Zirconium source: The molar ratio of the complexing agent is 1: (2-3);

[0054] Zirconium source: The molar ratio of the silicon source is (0.5-2): 1;

[0055] Zirconium source: The amount ratio of the auxiliary solvent is (0.01-0.04) mol: (20-25) mL;

[0056] Catalyst: The amount ratio of silicon source is (0.01-0.04) mol: (0.8-2) mL.

[0057] In the preparation of the precursor gel fibers, the precursor sol spinning liquid described in the syringe is used, and aluminum foil, release paper, nonwoven fabric or silicone paper are taken as the collection device.

[0058] In the acquisition of the ceramic fiber material, the parameters of the drying treatment, and the sintering treatment are:

[0059] Dry treatment: temperature is 50-80 ° C, time is 1-2 h;

[0060] Sintering treatment: The sintering temperature is 800-1400 ° C, the holding time is 1-2 hours, the temperature increase rate is 2-5 ° C / min, the cooling rate is the inert gas applied in the furnace cold and sintered into an AR atmosphere or N2 atmosphere.

[0061] A product, the product is the final product produced by a method of preparing a Si-Zr-C-C-Class american material.

[0062] An application of a product, the application of the product refers to the application of the final product obtained in the insulation.

[0063] The principles of the invention are described below:

[0064] The formulation process of the spinning censoon solution in the present invention is preferably comprised of the following steps: first soluble solute (e.g., PVP), placed in a beaker, add auxiliary solvent (such as anhydrous ethanol) and catalyst (eg, nitric acid) , Then stirring (magnetic stirring, glass rod stirring or shocking), dispersion (ultrasonic dispersion or mechanical dispersion), to make the solution soluble uniformly dispersion, thereby obtaining a spinning auxiliary solution.

[0065] The phases in the ceramic fiber material acquired in the present invention include ZrO2 phase and the SiC phase. Among them, ZrO2 phase has a very low solid thermal conductivity, but the infrared shielding capacity at high temperatures is very poor, and the solid thermal conductivity of SiC is high, but high temperature infrared shielding ability is excellent. Thus, the present invention combines the advantages of both, complement, so that the final product has a low thermal conductivity and a good high temperature infrared shielding capability.

[0066] Each material according to the present invention and the simply referred to as: polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polyvinyl glycol (PEG), polyoxyne alcohol (PEO ), Zirconate (Zr (OC4H9) 4), tetra-propoxy zirconium Zr (ONPR) 4, orthodoxate (TEOS), vinyl trimethoxysilane (VTMS), methyl triethoxide Silane (MTES), dimethyl diethoxysilane (DMDES), polymethylphenylsiloxane (PMPS), acetic acid (CH3COOH)), dimethylformamide (DMF).

[0067] The agitation time required for hydrolyzing and polycondensation in the present invention is 0.5 h-2 h.

[0068] The process parameters of the electrostatic spinning in the present invention are as follows: the voltage range is from 10 to 20 kV, the injection rate is 1-1.5 ml / hr, the receiving distance is 10-15 cm, the spinning environment is 20-40 ° C, spinning environment The humidity is 20-70%;

Example Embodiment

[0069] Example 1:

[0070] Precursor Sol Spinning Liquid: Weigh 1.91 g of a zirconate butyl icyster solution in a acetic acid solution of zirconate, continuously stirring to form a uniform solution, obtain a solution; place 0.25 g of PVP in a beaker, add 4.75 g of anhydrous ethanol and 0.5 g of 1 mol / L of dilute nitric acid, magnetic force for 1 hour, and ultrasonic 10 minute, so that PVP is well dispersed uniform, obtains a spinning auxiliary solution; add a solution and 0.74 g of VTMS to spinning In the auxiliary solution, stirring was stirred at room temperature for 30 minutes, resulting in sufficient hydrolysis and polycondensation of the zirconium source and silicon source to form a precursor sol spun liquid;

[0071] Preparation: Preparation of preparation precursor sol spun liquid into medical syringe, electrospinning technology, voltage is 20 kV, the injection rate is 1.5 ml / hr, the received distance is 15cm, spinning The ambient temperature is 30 ° C, the wet environment is 30%, and uniform precursor gel fibers can be obtained on the collection device;

[0072] Ceramic fiber material acquisition: first place the precursor gel fibers that are peeled from the collecting device in the blast drying tank, the temperature is 60 ° C, the time is 1 h; then the dry fiber is an AR atmosphere in an inert gas The sintering is performed, the sintering temperature is 1000 ° C, the holding time is 1 hour, the temperature rise rate is 2 ° C / min, and finally, the cooling rate is cold to obtain the final product.

Example Embodiment

[0073] Example 2:

[0074] Precursor Sol Spinning Liquid: Weigh 1.91 g of a zirconate butyl icyster solution in a acetic acid solution of zirconate, continuously stirring to form a uniform solution, obtain a solution; place 0.25 g of PVP in a beaker, add 4.75 g of anhydrous ethanol and 0.5 g of 1 mol / L of dilute nitric acid, magnetic force for 1 hour, and ultrason for 10 minutes, which allows PVP to be well dispersed uniform, obtain a spinning auxiliary solution; add a solution and 1.48g VTMS to spinning In the auxiliary solution, stirring was stirred at room temperature for 30 minutes, resulting in sufficient hydrolysis and polycondensation of the zirconium source and silicon source to form a precursor sol spun liquid;

[0075] Preparation: Put the prepared precursor sol spun liquid into the medical syringe, using electrostatic spinning techniques, voltage is 20 kV, the injection rate is 1.5 ml / hr, the reception distance is 15cm, spinning The wire ambient temperature is 30 ° C, the spinning environment is 30%, and uniform precursor gel fibers are obtained on the collection device;

[0076] Ceramic fiber material acquisition: first placed the precursor gel fibers from being peeled from the collecting device in the blast drying tank, the temperature is 60 ° C, the drying time is 1 h; then the dry fiber is in an inert gas The AR atmosphere was sintered, the sintering temperature was 1000 ° C, the holding time was 1 hour, the temperature increase rate was 2 ° C / min, and finally, the cooling rate was cold to obtain the final product.

[0077] Depend on figure 1 It can be seen that the thermal stability of the final product Si-Zr-O-C based ceramic fiber material is better.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Login to view more

PUM

Property	Measurement	Unit
Size diameter	<= 2.0	µm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Login to view more

Classification and recommendation of technical efficacy words

Low thermal conductivity
Improve barrier effect

People also interested in

Improve insulation effect Strong mechanical properties Ceramic materials

Preparation method of Si-Zr-O-C-based ceramic fiber material, product and application

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Preparation method for low-carbon aluminum-silicon-carbide carbon brick

Preparation method of titanium and titanium alloy wires or powder for 3D printing

High-strength vacuum insulation plate

Fireproof coating for thick formed steel constructions

Foamed plastic powder/expanded perlite flame-retardant and heat-insulating composite material

Classification and recommendation of technical efficacy words

High temperature resistant insulation for pipe

Foam concrete block manufactured by chemical foaming and manufacture method thereof

SiO2 enriched nano composite heat preserving and thermal insulating paste and preparing process thereof

Block aerogel composite material and preparation method thereof

Foam/Aerogel Composite Materials for Thermal and Acoustic Insulation and Cryogen Storage

Degradable non-woven fabric glue dipping composite preparation technology and materials thereof

Explosion-proof heat-insulation TPU film for automobile glass, and preparation method thereof

Chemical barrier fabric

Composite back panel of solar cell and preparation process of composite back panel

Underground coal mine explosion-proof method

People also interested in