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Preparation method for lanthanum zirconate ceramic fiber blanket

A technology of ceramic fiber felt and lanthanum zirconate, which is applied in the field of preparation of lanthanum zirconate ceramic fiber felt, can solve the problems of difficult large-scale production of electrospinning technology and poor fiber flexibility, and achieve easy control of microstructure and heat insulation Excellent performance and smooth surface effect

Active Publication Date: 2014-03-19
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few reports on lanthanum zirconate ceramic fibers. Zirconium oxychloride and lanthanum nitrate are used as precursors, polyvinylpyrrolidone (PVP) is used as spinning aid, gel fibers are prepared by electrospinning technology, and then calcined to obtain burnt green Stone type La 2 Zr 2 o 7 Nanofibers, whose fibers are connected by irregular nanosheets, resulting in poor fiber flexibility, see Mater.Sci.Engineer.:B2006,133,209-212; J.Nanosci.Nanotech.2011,11,2514-2519; Furthermore, since La 2 Zr 2 o 7 The material itself is difficult to sinter and its melting point is too high (2300 ° C), it is difficult to form fibers by traditional resistance melt blowing, and it is difficult to carry out large-scale production of electrospinning technology, which seriously hinders electrospinning La 2 Zr 2 o 7 Application of ceramic fiber in the field of heat insulation

Method used

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  • Preparation method for lanthanum zirconate ceramic fiber blanket
  • Preparation method for lanthanum zirconate ceramic fiber blanket
  • Preparation method for lanthanum zirconate ceramic fiber blanket

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Preparation of spinnable precursor sol

[0043] Add 49g of anhydrous lanthanum chloride to the acetic acid solution of 112g zirconium acetate (ZrO 2 Mass fraction 22%, containing ZrO 2 24.64g), stirred until the solution was clear and transparent, and then aged in a water bath at 40°C until the viscosity was 86Pa·s (viscosity was measured at room temperature with a rotational viscometer), to obtain a spinnable precursor sol;

[0044] (2) Centrifugal fiber formation to prepare gel fibers

[0045] The spinnable precursor sol prepared in step (1) is centrifuged into fibers, and the process conditions are: the diameter of the spinning hole is 0.3mm, the rotation speed of spinning is 6000r / min, the ambient temperature is 25°C, and the relative humidity is 30%. , get gel fiber, such as attached figure 1 shown;

[0046] (3) Gel fiber is collected into felt

[0047] Put the gel fiber evenly in the screen-like mold, then cover the mold with a screen, and then blow it ev...

Embodiment 2

[0052] As described in Example 1, the difference is:

[0053] In step (1), 49g of anhydrous lanthanum chloride was replaced with 86.6g of lanthanum nitrate hexahydrate, and aged to a viscosity of 164Pa·s.

[0054] In the step (2), the spinning speed is 9000r / min, the ambient temperature is 35°C, and the relative humidity is 20%.

[0055] Step (3) is the same as in Example 1.

[0056] In step (4), the technical conditions for the ceramicization of the gel fiber felt are: the temperature rises from room temperature to 600°C at a heating rate of 1°C / min, keeps at this temperature for 2 hours, and then rises to 900°C at a heating rate of 8°C / min , kept at this temperature for 1h to obtain a ceramic fiber felt, La 2 Zr 2 o 7 It is fluorite type; finally, the temperature is raised to 1200 °C at a rate of 20 °C / min, and kept at this temperature for 1 hour to obtain pyrochlore type La 2 Zr 2 o 7 Ceramic fiber felt.

[0057] The XRD picture of the gel fiber calcined to 900°C is...

Embodiment 3

[0060] As described in Example 1, the difference is:

[0061] The acetic acid solution quality of zirconium acetate in step (1) is 97.5g (ZrO 2 Mass fraction 22%, containing ZrO 2 21.45g).

[0062] In the step (2), the spinning speed is 7000r / min, the ambient temperature is 30°C, and the relative humidity is 40%.

[0063] Step (3) is the same as in Example 1.

[0064] In step (4), the process conditions for the ceramicization of the gel fiber mat are as follows: from room temperature to 600°C at a heating rate of 3°C / min, kept at this temperature for 2 hours, and then raised to 900°C at a heating rate of 8°C / min , kept at this temperature for 1h to obtain a ceramic fiber felt, La 2 Zr 2 o 7 It is fluorite type; finally, the temperature is raised to 1200 °C at a rate of 20 °C / min, and kept at this temperature for 1 hour to obtain pyrochlore type La 2 Zr 2 o 7 Ceramic fiber felt.

[0065] The XRD picture of the gel fiber calcined to 1200°C is attached Figure 4 As sho...

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Abstract

The invention relates to a preparation method for a lanthanum zirconate ceramic fiber blanket. The method uses lanthanum zirconate as the zirconium source, and lanthanum nitrate and lanthanum chloride and corresponding hydrate thereof as the lanthanum source, prepares precursor sol according to the molar ratio of La<3+>:Zr<4+> = 1:(0.87-1.15), and obtains gelatinous fiber through centrifugal fiber formation technology after aging; the gelatinous fiber is made into a gelatinous fiber blanket through cotton collecting and blanket forming; the La2Xr2O7 ceramic fiber blanket of pyrochlore type is obtained after calcination. The La2Xr2O7 ceramic fiber blanket of pyrochlore type, prepared by the invention, has a flat surface, is low in shot content, good in resilience, has a heat conductivity coefficient of 0.037-0.056W / (m*K), and has an excellent heat-insulating property; the method reduces the calcination temperature, and is simple in structure, controllable in technology, and suitable for large-scale production of the lanthanum zirconate ceramic fiber blanket.

Description

technical field [0001] The invention relates to a preparation method of lanthanum zirconate ceramic fiber felt, which belongs to the field of inorganic non-metallic materials. Background technique [0002] Ceramic fiber felt is the most common refractory ceramic fiber product. It has excellent machinability, good thermal stability and thermal shock resistance, and has the characteristics of low thermal conductivity, small heat capacity and high compressive strength. It is widely used in metallurgy, machinery, petroleum, etc. , chemical industry, ceramics, electronics and other fields, such as craft kiln lining, high temperature thermal equipment insulation, kiln baffle, etc. [0003] At present, my country's refractory ceramic fibers are developing rapidly, and new ceramic fibers and products such as aluminum silicate fibers, polycrystalline mullite fibers, polycrystalline alumina fibers, and zirconia fibers have been successfully developed, which basically meet the requirem...

Claims

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Application Information

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IPC IPC(8): D04H1/4209C03B37/04D04H1/46
Inventor 陈代荣李月明焦秀玲
Owner SHANDONG UNIV
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