CN109868526B - Method for preparing yttrium zirconate nanofiber by using zirconium-yttrium polymer precursor - Google Patents
Method for preparing yttrium zirconate nanofiber by using zirconium-yttrium polymer precursor Download PDFInfo
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Abstract
The invention relates to a method for preparing yttrium zirconate nano-fiber by using a zirconium-yttrium polymer precursor, which comprises the following steps: preparing a spinning solution by taking a zirconium-yttrium acetylacetone polymer as a precursor, absolute ethyl alcohol as a solvent and polyethylene oxide as a spinning auxiliary agent; carrying out electrostatic spinning on the spinning solution to obtain PAY-Z precursor fiber; and carrying out heat treatment on the PAY-Z precursor fiber to obtain the yttrium zirconate nanofiber. The yttrium zirconate fiber prepared by the invention has uniform diameter, compact structure and good flexibility, and can be used as a structure reinforcing material, a flexible luminous substrate, a high-temperature refractory material, a catalyst carrier and the like.
Description
Technical Field
The invention relates to a method for preparing yttrium zirconate (Y) by using a zirconium-yttrium polymer precursor2Zr2O7) A method of fiber belongs to the field of preparation of new ceramic fiber materials.
Background
Rare earth zirconates are a very versatile class of materials. The composite material has excellent performances of high melting point, high chemical stability, high ionic conductivity, low thermal conductivity, high catalytic activity and the like, and is widely applied to the fields of refractory materials, thermal barrier coatings, catalysis, photoluminescence, solid electrolytes, radioactive nuclear waste treatment and the like. Yttrium as a rare earth with a large reserve, yttrium zirconate (Y) is a very important property, both in terms of cost and availability of raw materials2Zr2O7) Has great advantages. The yttrium zirconate is in a cubic phase and defect state fluorite structure, and is widely applied to the fields of catalysis, photoluminescence, thermal barrier coatings, refractory materials, information detection, laser media, high-temperature windows and the like.
The current research on yttrium zirconate is mainly focused on powder and transparent ceramics, and the research on yttrium zirconate nano-fibers is not reported at present. The research on yttrium zirconate powder is mainly focused on the fields of photoluminescence and catalysis, and the research on transparent ceramics is mainly focused on the fields of high-refractive-index materials and scintillating materials. Such as: marc Jovanai et al used Pr and Fe co-doped yttrium zirconate in Ceramic pigments (Journal of the European Ceramic Society 38(2018) 2210-); the research on methane reforming catalysis using yttrium zirconate as a catalyst carrier (Journal of Energy Chemistry 25(2016) 825-; saif, M uses rare earth doped yttrium zirconate as phosphor material for information detection (Journal of Luminescence 135(2013) 187-195); chinese patent documents CN106927502A, CN107082449A and the like disclose various methods for preparing yttrium zirconate powder for photocatalysis; chinese patent document CN102557624A discloses a preparation method of yttrium zirconate transparent ceramic. The yttrium zirconate material is mainly prepared by a solid-phase reaction, a coprecipitation method and a sol-gel-combustion method, wherein the solid-phase reaction temperature is high, and the yttrium zirconate material is not suitable for preparing nano fibers; a coprecipitation method cannot obtain a uniform precursor, and the preparation of the nanofiber is difficult to realize; the sol-gel combustion method is also difficult to use for preparing nanofibers because it generates heat violently during combustion, which destroys the structure of the fibers. Due to the high melting point of yttrium zirconate, it is difficult to prepare yttrium zirconate into a fiber form by a melting method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing yttrium zirconate nano-fibers by using a zirconium-yttrium polymer precursor. The invention explores the zirconium-yttrium precursor, determines the zirconium-yttrium precursor suitable for preparing the fiber, and explores the electrostatic spinning condition and the sintering process to successfully prepare the yttrium zirconate fiber finally. The invention firstly prepares a zirconium-yttrium polymer precursor with high oxide content, and spins the zirconium-yttrium polymer precursor into yttrium zirconate nano-fibers with different diameters.
The technical scheme of the invention is as follows:
a method for preparing yttrium zirconate nano-fibers by using a zirconium-yttrium polymer precursor comprises the following steps:
preparing a spinning solution by using a zirconium-yttrium acetylacetone polymer (PAY-Z) as a precursor, absolute ethyl alcohol as a solvent and polyethylene oxide (PEO) as a spinning auxiliary agent;
carrying out electrostatic spinning on the spinning solution to obtain PAY-Z precursor fiber;
and carrying out heat treatment on the PAY-Z precursor fiber to obtain the yttrium zirconate nanofiber.
According to the invention, the preferred mass ratio of PAY-Z, absolute ethyl alcohol and PEO is as follows: 50-170: 200-700: 0.5-2; further preferably 60 to 150:250 to 625:0.5 to 1.5.
According to the invention, the preferred electrospinning conditions are:
performing electrostatic spinning on the spinning solution in an environment with the humidity of 20-65%, wherein the spinning voltage is 10-25 KV, the distance from a needle head to a receiving screen is 10-30 cm, and the propelling speed of a propelling pump is 0.008-0.04 mL/min;
further preferably, the spinning environment humidity is: 35 to 60 percent.
According to the invention, the heat treatment is preferably carried out in the air, the heat treatment time is 1-12 h, and the heat treatment temperature is 600-1200 ℃.
According to the invention, the zirconium-yttrium acetylacetone polymer precursor is synthesized by the following method:
dissolving zirconium oxychloride octahydrate and yttrium chloride hexahydrate into absolute methanol according to the molar ratio of 1:1, sequentially adding acetylacetone and triethylamine according to the molar ratio of 1: 1.1-4: 3.5-6.2 of the zirconium oxychloride octahydrate to the acetylacetone to the triethylamine, stirring for 3-5 h, and drying the solution under reduced pressure to obtain a zirconium-yttrium polymer precursor containing triethylamine hydrochloride;
soaking a zirconium-yttrium polymer precursor containing triethylamine hydrochloride in acetone, standing for 24-144 h, filtering to remove triethylamine hydrochloride, concentrating the filtrate under reduced pressure, and drying to obtain the zirconium-yttrium acetylacetone polymer precursor.
According to the preparation method of the poly-zirconium-yttrium precursor, the mol ratio of the zirconium oxychloride octahydrate to the acetylacetone to the triethylamine is preferably 1: 1.5-3: 4.3-6, 1500-4000 g of anhydrous methanol is added into each mol of the zirconium oxychloride octahydrate, the reduced pressure concentration and drying temperature is 30-40 ℃, and the acetone is calculated by adding 3000-5000 mL of acetone into each mol of the zirconium oxychloride octahydrate.
The yttrium zirconate fiber prepared by the invention has uniform diameter, compact structure and good flexibility, and can be used as a structure reinforcing material, a flexible luminous substrate, a high-temperature refractory material, a catalyst carrier and the like.
The invention has the technical characteristics and excellent effects that:
1. the invention provides a preparation scheme of the yttrium zirconate fiber for the first time, and the diameter of the prepared yttrium zirconate fiber is controllable.
2. The precursor of the zirconium-yttrium acetylacetone polymer prepared by the invention has stable property and can be preserved for a long time; the spinning solution prepared by the method is clear and transparent, and does not generate turbidity after being placed for a long time.
3. The zirconium-yttrium acetylacetone polymer precursor prepared by the invention has high oxide content, and the prepared fiber has uniform diameter, compact structure and good flexibility.
4. The invention does not need complex heat treatment process and atmosphere protection, has simple preparation process and is easy for batch production.
Drawings
FIG. 1 is an XRD pattern of yttrium zirconate fibers prepared in example 1.
FIG. 2 is an SEM image of yttrium zirconate fibers prepared in example 1.
FIG. 3 is an optical photograph of the yttrium zirconate fiber prepared in example 1.
Detailed Description
The present invention will be further described with reference to the following detailed description and accompanying drawings, but is not limited thereto.
The starting materials used in the examples are commercially available and were not further processed.
Example 1
A method for preparing yttrium zirconate fibers by taking a zirconium-yttrium polymer as a precursor comprises the following preparation steps:
(1) dissolving 1mol of zirconium oxychloride octahydrate and 1mol of yttrium chloride hexahydrate in 2000g of anhydrous methanol, respectively and sequentially adding 210g of acetylacetone and 500g of triethylamine (the molar ratio of the zirconium oxychloride octahydrate to the acetylacetone to the triethylamine is 1:2.1:4.9) after complete dissolution, and stirring for 5 hours to obtain a yellow solution;
(2) transferring the yellow solution obtained in the step (1) into a round-bottom flask, and carrying out reduced pressure concentration and drying at 40 ℃ to obtain a zirconium-yttrium polymer precursor containing triethylamine hydrochloride;
(3) and (3) soaking the zirconium-yttrium polymer precursor containing triethylamine hydrochloride obtained in the step (2) in 4000mL of acetone, standing at room temperature for 72h, and filtering triethylamine hydrochloride to obtain a zirconium-yttrium polymer precursor acetone solution which is clear, transparent and bright yellow.
(4) Decompressing, concentrating and drying the zirconium-yttrium precursor polymer acetone solution in the step (3) at 40 ℃ to obtain a zirconium-yttrium acetylacetone polymer precursor;
(5) dissolving 9g of the zirconium-yttrium acetylacetone polymer precursor obtained in the step (4) into 20g of absolute ethyl alcohol, adding 50mg of polyoxyethylene after the zirconium-yttrium acetylacetone polymer precursor is completely dissolved, stirring, and continuing stirring for 2 hours after the polyoxyethylene is completely dissolved to obtain a clear and transparent precursor spinning solution;
(6) performing electrostatic spinning on the precursor spinning solution obtained in the step (5) under the voltage of 15KV to obtain zirconium-yttrium polymer precursor fibers; the electrostatic spinning humidity is 45%, the distance from the needle head to the receiving screen is 25cm, and the propelling speed of the propelling pump is 0.02 mL/min;
(7) and (3) treating the precursor fiber spun in the step (6) at 1000 ℃ for 2h in the air to obtain the yttrium zirconate nanofiber, wherein the fiber has a compact structure, good flexibility and uniform diameter (about 500 nm).
Example 2
As described in example 1, except that:
in the step (1), 1mol of zirconium oxychloride octahydrate and 1mol of yttrium chloride hexahydrate are dissolved in 2000g of anhydrous methanol, 150g of acetylacetone and 435g of triethylamine (the molar ratio of zirconium oxychloride octahydrate to acetylacetone to triethylamine is 1:1.5:4.3) are respectively and sequentially added after complete dissolution, and a yellow solution is obtained after stirring for 5 hours.
Example 3
As described in example 1, except that:
in the step (1), 1mol of zirconium oxychloride octahydrate and 1mol of yttrium chloride hexahydrate are dissolved in 2000g of anhydrous methanol, 300g of acetylacetone and 607g of triethylamine (the molar ratio of zirconium oxychloride octahydrate to acetylacetone to triethylamine is 1:3:6) are respectively and sequentially added after complete dissolution, and a yellow solution is obtained after stirring for 5 hours.
Example 3
As described in example 1, except that:
and (3) soaking the zirconium-yttrium polymer precursor containing triethylamine hydrochloride obtained in the step (2) in 4000mL of acetone, standing at room temperature for 48h, and filtering triethylamine hydrochloride to obtain an acetone solution of the zirconium-yttrium polymer precursor.
Example 4
As described in example 1, except that:
and (3) soaking the zirconium-yttrium polymer precursor containing triethylamine hydrochloride obtained in the step (2) in 4000mL of acetone, standing at room temperature for 100h, and filtering triethylamine hydrochloride to obtain an acetone solution of the zirconium-yttrium polymer precursor.
Example 5
As described in example 1, except that:
dissolving 6g of the zirconium-yttrium polymer precursor obtained in the step (4) into 20g of absolute ethyl alcohol, adding 50mg of polyoxyethylene after the zirconium-yttrium polymer precursor is completely dissolved, stirring, and continuing stirring for 2h after the polyoxyethylene is completely dissolved to obtain a clear and transparent precursor spinning solution;
performing electrostatic spinning on the precursor spinning solution obtained in the step (5) under the voltage of 20KV as described in the step (6) of the embodiment 1, wherein the electrostatic spinning humidity is 50%, the distance from a needle head to a receiving screen is 15cm, and the propelling speed of a propelling pump is 0.03 mL/min; obtaining the zirconium-yttrium polymer precursor fiber.
Example 6
As described in example 1, except that:
dissolving 12g of the zirconium-yttrium polymer precursor obtained in the step (4) into 50g of absolute ethyl alcohol, adding 150mg of polyoxyethylene after the zirconium-yttrium polymer precursor is completely dissolved, stirring, and continuing stirring for 2h after the polyoxyethylene is completely dissolved to obtain a clear and transparent precursor spinning solution;
performing electrostatic spinning on the precursor spinning solution obtained in the step (5) under the voltage of 20KV as described in the step (6) of the embodiment 1, wherein the electrostatic spinning humidity is 30%, the distance from a needle head to a receiving screen is 20cm, and the propelling speed of a propelling pump is 0.01 mL/min; obtaining the zirconium-yttrium polymer precursor fiber.
Example 7
As described in example 1, except that:
dissolving 15g of the zirconium-yttrium polymer precursor obtained in the step (4) into 25g of absolute ethyl alcohol, adding 150mg of polyoxyethylene after the zirconium-yttrium polymer precursor is completely dissolved, stirring, and continuing stirring for 2h after the polyoxyethylene is completely dissolved to obtain a clear and transparent precursor spinning solution;
and (3) performing electrostatic spinning on the precursor spinning solution obtained in the step (5) at a voltage of 15KV to obtain the zirconium-yttrium polymer precursor fiber as described in the step (6) of the example 1.
Example 8
As described in the step (7) of the embodiment 1, the precursor fiber spun in the step (6) is treated at 600 ℃ for 12h in the air to obtain the pure-phase yttrium zirconate nanofiber, and the pure-phase yttrium zirconate nanofiber has good flexibility, uniform diameter, fine grains and high strength.
Comparative example 1
As described in step (1) of example 1, 1mol of zirconium oxychloride octahydrate and 1mol of yttrium chloride hexahydrate were dissolved in 2000g of anhydrous methanol, and after complete dissolution, 210g of acetylacetone and 650g of triethylamine (molar ratio of zirconium oxychloride octahydrate: acetylacetone: triethylamine: 1:2.1:6.4) were added in this order, followed by stirring for 5 hours to obtain a yellow solution;
compared with the example 1, the zirconium-yttrium polymer acetone solution containing triethylamine hydrochloride is difficult to filter, and the obtained zirconium-yttrium polymer precursor has higher impurity content. It can be seen that too high triethylamine content can introduce too many impurities, which affects the quality of yttrium zirconate nanofibers.
Comparative example 2
As described in step (1) of example 1, 1mol of zirconium oxychloride octahydrate and 1mol of yttrium chloride hexahydrate were dissolved in 2000g of anhydrous methanol, and after complete dissolution, 100g of acetylacetone and 500g of triethylamine (molar ratio of zirconium oxychloride octahydrate: acetylacetone: triethylamine: 1:0.99:4.9) were added in this order, followed by stirring for 5 hours to obtain a yellow solution;
compared with the embodiment 1, the content of acetylacetone is too low, the stability of the precursor spinning solution is reduced, and slight hydrolysis is caused after long-term storage, so that the spinning performance of the precursor is influenced.
Comparative example 3
Soaking the zirconium-yttrium polymer precursor containing triethylamine hydrochloride obtained in the step (2) in 4000mL of acetone, standing at room temperature for 12 hours, and then filtering off triethylamine hydrochloride to obtain an acetone solution of the zirconium-yttrium polymer precursor, wherein the acetone solution is clear and transparent and has bright yellow color, as described in the step (3) of the example 1.
Compared with the embodiment 1, the obtained zirconium-yttrium polymer precursor containing triethylamine hydrochloride has the advantages that the standing time is too short, the spinnability of the precursor is reduced, and triethylamine hydrochloride serving as an impurity is separated out from the surface of the precursor fiber.
Comparative example 4
Dissolving 3g of the zirconium-yttrium polymer precursor obtained in the step (4) into 20g of absolute ethyl alcohol, adding 50mg of polyoxyethylene after the zirconium-yttrium polymer precursor is completely dissolved, stirring, and continuing stirring for 2h after the polyoxyethylene is completely dissolved to obtain a clear and transparent precursor spinning solution as described in the step (5) of the example 1;
performing electrostatic spinning on the precursor spinning solution obtained in the step (5) at a voltage of 25KV to obtain zirconium-yttrium polymer precursor fibers as described in the step (6) of the example 1;
compared with example 1, the fiber diameter is thinner, but the fiber diameter is not uniform, and slag balls exist. It can be seen that the zirconium-yttrium polymer precursor content is too low, and although the fibers can be spun, the fibers after heat treatment have non-uniform diameters and shot.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the invention, and these modifications and improvements should be considered within the scope of the invention.
Claims (8)
1. A method for preparing yttrium zirconate nano-fibers by using a zirconium-yttrium polymer precursor comprises the following steps:
preparing a spinning solution by using a zirconium-yttrium acetylacetone polymer PAY-Z as a precursor, absolute ethyl alcohol as a solvent and polyethylene oxide (PEO) as a spinning auxiliary agent; the mass ratio of the PAY-Z, the absolute ethyl alcohol and the PEO is as follows: 50-170: 200-700: 0.5-2;
carrying out electrostatic spinning on the spinning solution to obtain PAY-Z precursor fiber;
carrying out heat treatment on the PAY-Z precursor fiber to obtain yttrium zirconate nano-fiber;
the zirconium-yttrium acetylacetone polymer precursor is synthesized by the following method:
dissolving zirconium oxychloride octahydrate and yttrium chloride hexahydrate into absolute methanol according to the molar ratio of 1:1, sequentially adding acetylacetone and triethylamine according to the molar ratio of 1: 1.1-4: 3.5-6.2 of the zirconium oxychloride octahydrate to the acetylacetone to the triethylamine, stirring for 3-5 h, and drying the solution under reduced pressure to obtain a zirconium-yttrium polymer precursor containing triethylamine hydrochloride;
soaking a zirconium-yttrium polymer precursor containing triethylamine hydrochloride in acetone, standing for 24-144 h, filtering to remove triethylamine hydrochloride, concentrating the filtrate under reduced pressure, and drying to obtain the zirconium-yttrium acetylacetone polymer precursor.
2. The method for preparing yttrium zirconate nanofibers according to claim 1, wherein the mass ratio of PAY-Z, absolute ethanol and PEO is as follows: 60-150: 250-625: 0.5-1.5.
3. The process for preparing yttrium zirconate nanofibers from zirconium-yttrium polymer precursor according to claim 1, wherein electrospinning is carried out under the following conditions:
the spinning solution is subjected to electrostatic spinning in an environment with the humidity of 20-65%, the spinning voltage is 10-25 KV, the distance from a needle head to a receiving screen is 10-30 cm, and the propelling speed of a propelling pump is 0.008-0.04 mL/min.
4. The process for preparing yttrium zirconate nanofibers according to claim 3, wherein the spinning environment humidity is: 35% -60%.
5. The method for preparing yttrium zirconate nanofibers according to claim 1, wherein the heat treatment temperature is 600-1200 ℃.
6. The method for preparing the yttrium zirconate nanofibers from the zirconium-yttrium polymer precursor according to claim 1, wherein the heat treatment is carried out in air for 1-12 hours.
7. The method for preparing yttrium zirconate nanofibers according to claim 1, wherein the molar ratio of zirconium oxychloride octahydrate to acetylacetone to triethylamine is 1: 1.5-3: 4.3-6.
8. The method for preparing yttrium zirconate nanofibers according to claim 1, wherein 1500-4000 g of anhydrous methanol is added per mole of zirconium oxychloride octahydrate, the concentration under reduced pressure and drying temperature is 30-40 ℃, and acetone is added in an amount of 3000-5000 mL per mole of zirconium oxychloride octahydrate.
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