A kind of preparation method of lanthanum zirconate ceramic fiber mat
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 difficulty in large-scale production of electrospinning technology, poor fiber flexibility, etc., and achieves easy control of microstructure and thermal insulation. Excellent performance and smooth surface
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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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