CN111978550A - Yttrium/aluminum-organic polymer precursor, yttrium aluminum garnet continuous fiber and preparation method - Google Patents

Yttrium/aluminum-organic polymer precursor, yttrium aluminum garnet continuous fiber and preparation method Download PDF

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CN111978550A
CN111978550A CN202010944335.4A CN202010944335A CN111978550A CN 111978550 A CN111978550 A CN 111978550A CN 202010944335 A CN202010944335 A CN 202010944335A CN 111978550 A CN111978550 A CN 111978550A
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yttrium
aluminum
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朱陆益
谢永帅
彭影
王新强
张光辉
许东
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Shandong University
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    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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Abstract

The invention relates to a yttrium/aluminum-organic polymer precursor, yttrium aluminum garnet continuous fiber and a preparation method thereof, wherein the preparation method comprises the steps of synthesizing and preparing the yttrium/aluminum-organic polymer precursor and preparing precursor spinning sol by the yttrium/aluminum-organic polymer precursor; and then preparing the precursor spinning sol into precursor continuous gel fiber by dry spinning, and carrying out heat treatment on the precursor continuous gel fiber to obtain the yttrium aluminum garnet continuous fiber. The invention firstly proposes that the yttrium/aluminum-organic polymer is used as a precursor to prepare the yttrium aluminum garnet fiber, the oxide content in the yttrium/aluminum-organic polymer precursor is more than 35 percent, and other components are not required to be added as spinning aids, thereby avoiding the treatment of the subsequent spinning aids. The yttrium aluminum garnet continuous fiber prepared by the method has the advantages of high purity, high strength, uniform and adjustable diameter, good flexibility, compact structure, no air holes, no cracks and other defects.

Description

Yttrium/aluminum-organic polymer precursor, yttrium aluminum garnet continuous fiber and preparation method
Technical Field
The invention relates to an yttrium/aluminum-organic polymer precursor, an yttrium aluminum garnet continuous fiber and a preparation method thereof, belonging to the field of preparation of special ceramic fibers.
Technical Field
Yttrium aluminum garnet (Y)3Al5O12YAG) fiber is a generation of high-performance ceramic fiber which is newer than alumina fiber, not only has the characteristics of high temperature resistance, high strength, high modulus, oxidation resistance, corrosion resistance, high temperature creep resistance, thermal shock resistance, excellent optical performance and the like of yttrium aluminum garnet, but also has the characteristics of large length-diameter ratio, good flexibility, winding or two-dimensional and three-dimensional weaving and the like of a continuous fiber material, and can be widely used as a high-temperature heat-insulating material, a structure-reinforcing material and a flexible optical material.
At present, the existing methods for preparing YAG fibers mainly comprise a melting method and a sol-gel method. The melting method is to melt yttrium oxide and aluminum oxide into liquid phase at high temperature, then spin the liquid phase into fiber to obtain YAG single crystal fiber (Journal of the European Ceramic Society,2002,22(11): 1831-1837). since the melting point of YAG is up to 1970 ℃, the method has high requirements on equipment and great process difficulty, and the prepared fiber has large diameter and short length, and is difficult to prepare YAG continuous fiber with the length of tens of meters or even hundreds of meters. The sol-gel method is characterized in that a spinnable precursor sol is synthesized by a chemical means, a gel fiber is prepared by a spinning process, and the YAG fiber is obtained by heat treatment of the gel fiber. Pullar et al (Journal of the European Ceramic Society,1999,19(9):1747-1758) produced YAG fibers having a diameter of 120 μm by a sol-gel method and a blow spinning process in combination with steam treatment, however, this method resulted in short fibers and failed to achieve continuous fiber production.
Chinese patent document CN102011215A discloses a process for preparing yttrium aluminum garnet-based continuous fiber by a sol-gel method, which uses yttrium aluminum garnet as a main component and adds a second component as a grain inhibitor. Adding inorganic aluminum salt, yttrium oxide, a grain inhibitor, acetic acid and metal aluminum into distilled water, and reacting the mixture solution under the conditions of continuous stirring and condensation reflux at a certain temperature to obtain yttrium aluminum garnet sol containing the grain inhibitor. Adding a certain amount of spinning auxiliary agent into the sol, and concentrating the solution to obtain the spinnable fiber precursor sol. And obtaining the yttrium aluminum garnet-based continuous fiber precursor containing the organic matters by adopting a dry method or a wet method for spinning. Drying and sintering the precursor to obtain the yttrium aluminum garnet-based fiber. However, the preparation process of the patent needs to add a grain inhibitor, which greatly reduces the purity of the fiber and the use temperature, and influences the product quality.
Chinese patent document CN105002601A discloses a polycrystalline Al2O3-Y3Al5O12The preparation method of the (YAG) complex phase fiber or the pure YAG fiber comprises the following preparation steps: (1) preparation of Al2O3-YAG complex phase fibres and YAG fibre precursor colloids; (2) centrifugal spinning: adopting a self-made centrifugal spinning machine to carry out centrifugal spinning to obtain gel fibers with uniform diameters at proper wind speed, rotation speed and relative humidity; (3) preparation of Al2O3-YAG complex phase fibre and YAG fibre: drying the obtained gel fiber at 55-75 ℃ for 12h, and then carrying out heat treatment at 800-1400 ℃ for 2h to obtain the required polycrystalline Al2O3-YAG complex phase fibres and YAG continuous fibres. The preparation method has a complex reaction process, and the fibers prepared by centrifugal spinning are short and have poor orderliness, so that the requirements of winding, weaving and the like cannot be met.
Chinese patent document CN106927808A discloses a method for preparing yttrium aluminum garnet continuous fiber, which utilizes Al-containing fiber13Preparing spinnable precursor sol from aluminum oxide sol, gamma-AlOOH nano dispersion liquid, yttrium oxide sol, glacial acetic acid and polyvinylpyrrolidone (PVP) of the colloidal particles, preparing gel continuous fibers by adopting a dry spinning technology, and performing heat treatment to obtain yttrium aluminum garnet continuous fibers with the diameter of 6-12 mu m. The fibers are relatively uniform in diameter but are madeIn the preparation process, the pH value needs to be adjusted to about 2.0 by using nitric acid, the requirement on the corrosion resistance of equipment is high, and the preparation cost is high.
In addition to the above methods, the continuous YAG fiber is prepared by using YAG powder as raw material, adding binder and plasticizer, ball milling under vacuum, extruding under high pressure, and sintering under vacuum, and has uniform diameter and high transparency, but the method has complex process and high requirement for equipment.
The invention content is as follows:
aiming at the defects of the prior art, the invention provides an yttrium/aluminum-organic polymer precursor, an yttrium aluminum garnet continuous fiber and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of yttrium/aluminum-organic polymer precursor comprises the following steps:
dissolving an aluminum source and an yttrium source in an organic solvent, adding acetylacetone, stirring for 1-5 hours, dropwise adding triethylamine, continuously stirring for 1-12 hours after dropwise adding, and drying at 25-40 ℃ under reduced pressure; and soaking the product in an extractant, standing for 12-144 hours, filtering, and drying the filtrate at 25-40 ℃ under reduced pressure to obtain the yttrium/aluminum-organic polymer precursor.
According to the invention, the aluminum source is one or a mixture of crystalline aluminum chloride and anhydrous aluminum chloride; the yttrium source is one or a mixture of crystalline yttrium chloride and anhydrous yttrium chloride.
According to a preferred embodiment of the present invention, the organic solvent is absolute methanol, absolute ethanol or N, N-Dimethylformamide (DMF).
According to the invention, the mol ratio of the aluminum source to the yttrium source to the acetylacetone to the triethylamine is 1: (0.5-0.7): (1.2-5.2): (2.4-9.6); further preferably, the mol ratio of the aluminum source to the yttrium source to the acetylacetone to the triethylamine is 1: 0.6: (1.28-3.2): (4-8).
According to the invention, the adding amount of the organic solvent is preferably controlled to be 500-1000 g per 100 g of the aluminum source.
According to the invention, the temperature of the reduced pressure drying is preferably 30-40 ℃.
According to the invention, the extracting agent is one or a mixture of acetone and tetrahydrofuran; the adding amount of the extracting agent is controlled to be 3000-3600 mL per mol of aluminum source, and the extracting time is 48-96 h.
According to the present invention, there is also provided an yttrium/aluminum-organic polymer precursor prepared as described above.
According to the invention, the preparation method of the yttrium aluminum garnet continuous fiber comprises the following steps:
dissolving an yttrium/aluminum-organic polymer precursor in an organic solvent, and obtaining precursor spinning sol after decompression and concentration; and preparing the precursor spinning sol into precursor continuous gel fiber through dry spinning, pretreating the precursor continuous gel fiber at 100-160 ℃, continuously heating to 800-1200 ℃ at the speed of 0.5-5 ℃/min, and preserving heat for 10-240 min to obtain the yttrium aluminum garnet continuous fiber.
According to a preferred embodiment of the present invention, the mass ratio of the yttrium/aluminum-organic polymer precursor to the organic solvent is 1: (3-4); further preferably, the organic solvent is absolute methanol, absolute ethanol or N, N-Dimethylformamide (DMF).
According to the invention, the temperature of the reduced pressure concentration is 30-65 ℃, and the viscosity of the precursor spinning sol after the reduced pressure concentration is 10-100 Pa.s at 20 ℃.
According to the invention, the dry spinning process is preferably as follows: and (2) loading the precursor spinning sol into a liquid material tank of a spinning device, defoaming in vacuum for 1.5-2.5 h, pressurizing the precursor spinning sol by a steel cylinder nitrogen or metering pump at the temperature of 10-40 ℃ and the relative humidity of 20-80% to 0.5 MPa, ejecting the precursor spinning sol from a spinneret plate hole with the aperture of 0.04-0.20 mm, and performing multistage drafting and filament collection to obtain the precursor continuous gel fiber with the diameter of 30-150 mu m.
According to the invention, the pretreatment is preferably carried out in a steam environment at 120-140 ℃ for 10-30 min.
According to the invention, preferably, the heating rate is 0.8-1.2 ℃/min, and the temperature is kept for 100-150 min; further preferably, the temperature rise rate is 1 ℃/min, and the temperature is kept for 120 min.
The invention also provides an yttrium aluminum garnet continuous fiber material prepared by the preparation method. The yttrium aluminum garnet continuous fiber material has the excellent characteristics of high purity, high strength, good flexibility, uniform and adjustable diameter, winding, weaving and the like, and the obtained continuous fiber has uniform internal crystal grain size, compact arrangement and no defects of pores, cracks and the like on the surface.
The invention has the technical characteristics and excellent effects that:
1. the invention firstly provides an yttrium/aluminum-organic polymer precursor and a method for preparing yttrium aluminum garnet continuous fibers by using the precursor, the content of oxides in the prepared yttrium/aluminum-organic polymer precursor is more than 35 percent, the content of the oxides in the precursor is greatly improved, other components are not required to be added to be used as spinning aids, and the subsequent processing of the spinning aids is avoided.
2. The yttrium/aluminum-organic polymer precursor prepared by the invention has stable property, does not deteriorate after long-term storage, and the spinning sol prepared by the yttrium/aluminum-organic polymer precursor is clear and transparent, and can be stored for a long time without precipitation, turbidity and other phenomena.
3. The yttrium aluminum garnet continuous fiber is prepared by adopting dry spinning, the technical parameters such as spinning pressure, drawing tension and the like can be regulated and controlled by arranging the spinneret plates with different apertures, the yttrium aluminum garnet continuous fiber material with adjustable diameter and uniform diameter distribution can be obtained to meet different application requirements, and in the preparation process of the yttrium aluminum garnet continuous fiber, the gas in precursor spinning sol can be promoted to slowly escape through pretreatment in steam, so that the final yttrium aluminum garnet continuous fiber product has compact microstructure, smooth surface, no pores or cracks and obviously improved strength.
4. The prepared yttrium aluminum garnet continuous fiber has the advantages of high purity, high strength, uniform and adjustable diameter, good flexibility, compact structure, no defects of air holes, cracks and the like, and has wide application prospect in the fields of high-temperature heat insulation materials, structure reinforcing materials, flexible optical materials and the like. The method has the characteristics of simplicity, low cost, no pollution and stable fiber quality, and is easy for industrial production.
Drawings
FIG. 1 photo of an optical photograph of the yttrium/aluminum-organic polymer precursor prepared in example 1.
FIG. 2 SEM image of YAG continuous fiber prepared in example 1.
FIG. 3 XRD pattern of yttrium aluminum garnet continuous fibers prepared in example 1.
Fig. 4 photo optics of the precursor spin sol continuous spinning process of example 2.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. At the same time, 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.
The raw materials used in the examples are all conventional commercial products.
Example 1
A preparation method of yttrium/aluminum-organic polymer precursor and yttrium aluminum garnet continuous fiber comprises the following steps:
(1) 423 g of anhydrous aluminum chloride and 577 g of crystallized yttrium chloride are dissolved in 3600 g of anhydrous methanol, 500 g of acetylacetone is added into the solution after complete dissolution, 3000 g of triethylamine is added dropwise after stirring for 2 hours, and stirring is continued for 2 hours after the dropwise addition is finished, so as to obtain a clear precursor solution;
(2) drying the precursor solution prepared in the step (1) at 38 ℃ under reduced pressure, adding 11 liters of acetone after the precursor solution is completely dried, sealing, standing and extracting for 144 hours to obtain acetone precursor extract and insoluble triethylamine hydrochloride;
(3) removing the triethylamine hydrochloride insoluble in the step (2) through reduced pressure suction filtration to obtain acetone precursor extract, and drying the extract at 32 ℃ under reduced pressure to obtain an yttrium/aluminum-organic polymer precursor;
(4) dissolving 100 g of yttrium/aluminum-organic polymer precursor prepared in the step (3) in 300 g of absolute ethyl alcohol, continuously stirring for 2 hours after complete dissolution to obtain a precursor spinning solution, and concentrating the precursor spinning solution at 32 ℃ until the viscosity is 80 Pa.s to obtain precursor spinning sol;
(5) loading the precursor spinning sol prepared in the step (4) into a liquid material tank of a spinning device, defoaming in vacuum for 2h at room temperature, and spraying the precursor spinning sol from a niobium-tantalum alloy spinneret plate with 50 holes and a diameter of 60 mu m under the conditions that the pressure is 2MPa, the ambient temperature is 30 ℃ and the relative humidity is 55% to obtain continuous and draftable precursor continuous gel fibers;
(6) and (3) preserving the heat of the precursor continuous gel fiber prepared in the step (5) for 20min in a steam environment at the temperature of 130 ℃, continuously heating to 1000 ℃ at the speed of 1 ℃/min, preserving the heat for 120min, and cooling along with a furnace to obtain the yttrium aluminum garnet continuous fiber.
An optical photograph of the yttrium/aluminum-organic polymer precursor prepared in this example is shown in FIG. 1.
The SEM and XRD patterns of the yttrium aluminum garnet continuous fiber prepared in this example are shown in fig. 2 and 3.
As can be seen from fig. 2 and 3, the yttrium aluminum garnet continuous fiber prepared in this example is compact and smooth, almost completely transparent, has a purity of 99.9%, a length of tens of meters or hundreds of meters, good continuity, good flexibility, crimpability, winding ability, uniform diameter, and a diameter of about 35 μm.
Example 2
As described in example 1, except that:
the step (5) is as follows: and (3) loading the precursor spinning sol prepared in the step (4) into a liquid material tank of a spinning device, defoaming in vacuum at room temperature for 2h, and spraying the precursor spinning sol from a niobium-tantalum alloy spinneret plate with 200 holes and a diameter of 60 mu m under the conditions that the pressure is 2MPa, the ambient temperature is 30 ℃ and the relative humidity is 55% to obtain the continuous and drawable precursor gel fiber.
Fig. 4 shows an optical photograph of the precursor spinning sol continuous spinning prepared in this example, and the yttrium aluminum garnet fiber obtained by using the spinning parameters of this example is compact, smooth, almost completely transparent, has a purity of 99.9%, a length of several tens of meters or more, and has a good continuity, a good flexibility, a crimpability, a winding ability, a uniform diameter of about 35 μm, and a better bundling property compared to example 1.
Example 3
As described in example 1, except that:
the step (5) is as follows: and (3) loading the precursor spinning sol prepared in the step (4) into a liquid material tank of a spinning device, defoaming in vacuum for 2h at room temperature, and spraying the precursor spinning sol from a niobium-tantalum alloy spinneret plate with 200 holes and the diameter of 40 mu m under the conditions that the pressure is 1.6MPa, the ambient temperature is 30 ℃ and the relative humidity is 55%, so as to obtain the continuous and drawable precursor gel fiber.
The yttrium aluminum garnet fiber prepared by the embodiment is compact and smooth, almost completely transparent, the purity can reach 99.9%, the length can reach dozens of meters or even hundreds of meters, the continuity is good, the flexibility is good, the fiber can be curled and wound, the diameter is uniform, the diameter is about 30 micrometers, and the fiber has better flexibility compared with the fiber prepared by the embodiment 1.
Example 4
As described in example 1, except that:
the step (4) is as follows: dissolving 100 g of the yttrium/aluminum-organic polymer precursor prepared in the step (3) in 300 g of absolute ethyl alcohol, continuously stirring for 2 hours after complete dissolution to obtain a precursor spinning solution, and concentrating the spinning solution at 32 ℃ until the viscosity is 100 Pa.s to obtain a precursor spinning sol;
the step (5) is as follows: and (3) loading the precursor spinning sol prepared in the step (4) into a liquid material tank of a spinning device, defoaming in vacuum at room temperature for 2h, and spraying the precursor spinning sol from a niobium-tantalum alloy spinneret plate with 20 holes and the diameter of 150 mu m under the conditions that the pressure is 2MPa, the ambient temperature is 30 ℃ and the relative humidity is 55% to obtain the continuous and drawable precursor gel fiber.
The yttrium aluminum garnet fiber prepared by the embodiment is compact and smooth, is almost transparent, has the purity of 99.9 percent, the length of tens of meters, good continuity, uniform diameter of about 90 mu m and certain flexibility.
Example 5
A method for preparing high-purity Yttrium Aluminum Garnet (YAG) continuous fibers by using an yttrium/aluminum-organic polymer as a precursor comprises the following steps:
(1) 423 g of anhydrous aluminum chloride and 577 g of crystallized yttrium chloride are dissolved in 3600 g of anhydrous methanol, 500 g of acetylacetone is added into the solution after the anhydrous aluminum chloride and the crystalline yttrium chloride are completely dissolved, 2500 g of triethylamine is added dropwise after the stirring for 2 hours, and the stirring is continued for 2 hours after the dropwise addition is finished, so as to obtain a clear precursor solution;
(2) drying the precursor solution prepared in the step (1) at 38 ℃ under reduced pressure, adding 11 liters of acetone after the precursor solution is completely dried, sealing, standing and extracting for 72 hours to obtain acetone precursor extract and insoluble triethylamine hydrochloride;
(3) removing the triethylamine hydrochloride insoluble in the step (2) through reduced pressure suction filtration to obtain acetone precursor extract, and drying the extract at 32 ℃ under reduced pressure to obtain an yttrium/aluminum-organic polymer precursor;
(4) dissolving 100 g of yttrium/aluminum-organic polymer precursor prepared in the step (3) in 300 g of absolute ethyl alcohol, continuously stirring for 2 hours after complete dissolution to obtain a precursor spinning solution, and concentrating the precursor spinning solution at 32 ℃ until the viscosity is 40 Pa.s to obtain precursor spinning sol;
(5) loading the precursor spinning sol prepared in the step (4) into a liquid material tank of a spinning device, defoaming in vacuum for 2h at room temperature, and spraying the precursor spinning sol from a niobium-tantalum alloy spinneret plate with 50 holes and a diameter of 60 mu m under the conditions that the pressure is 1.6MPa, the ambient temperature is 30 ℃ and the relative humidity is 55% to obtain continuous and draftable precursor continuous gel fibers;
(6) and (3) preserving the heat of the precursor continuous gel fiber prepared in the step (5) for 30min in a steam environment at the temperature of 130 ℃, continuously heating to 1000 ℃ at the speed of 1 ℃/min, preserving the heat for 120min, and cooling along with a furnace to obtain the yttrium aluminum garnet continuous fiber.
The precursor prepared by the embodiment is slightly poorer in spinnability than that of embodiment 1, but the obtained yttrium aluminum garnet fiber is still compact and smooth in surface, the fiber is still almost transparent in macroscopic view, the purity can reach 99.9%, the flexibility is good, and the diameter is distributed at 30-40 microns.
Comparative example 1
As described in example 1, except that:
the step (1) is as follows: 423 g of anhydrous aluminum chloride and 577 g of crystalline yttrium chloride are dissolved in 3600 g of anhydrous methanol, 500 g of acetylacetone is added into the solution after complete dissolution, 3000 g of triethylamine is directly added after stirring for 2 hours, and stirring is continued for 2 hours after dropwise addition is finished, so that turbid precursor solution is obtained.
The yttrium/aluminum-organic polymer precursor prepared by the comparative example has poor polymerizability and can hardly be used for spinning, which shows that the addition speed of triethylamine influences the spinnability of the yttrium/aluminum-organic polymer precursor.
Comparative example 2
As described in example 1, except that:
the step (6) is as follows: and (3) heating the precursor continuous gel fiber prepared in the step (5) to 1000 ℃ at the speed of 1 ℃/min, preserving the temperature for 120min, and cooling along with a furnace to obtain the yttrium aluminum garnet continuous fiber.
The yttrium aluminum garnet continuous fiber prepared by the comparative example has low strength and slight pulverization, and the surface cracks and air holes of the fiber are more seen microscopically, which indicates that the steam pretreatment is an essential process step for obtaining high-quality yttrium aluminum garnet continuous fiber.
Comparative example 3
As described in example 1, except that:
the step (6) is as follows: and (3) heating the precursor continuous gel fiber prepared in the step (5) to 1000 ℃ at a speed of 100 ℃/min, keeping the temperature for 120min, and cooling along with the furnace to obtain the yttrium aluminum garnet continuous fiber.
The yttrium aluminum garnet continuous fiber prepared by the comparative example has more pores, lower strength and poorer flexibility, which shows that the high temperature rise speed in the heat treatment process is not favorable for obtaining high-quality yttrium aluminum garnet continuous fiber.

Claims (10)

1. A preparation method of yttrium/aluminum-organic polymer precursor comprises the following steps:
dissolving an aluminum source and an yttrium source in an organic solvent, adding acetylacetone, stirring for 1-5 hours, dropwise adding triethylamine, continuously stirring for 1-12 hours after dropwise adding, drying at 25-40 ℃ under reduced pressure, soaking the product in an extracting agent, standing for 12-144 hours, filtering, and drying the filtrate at 25-40 ℃ under reduced pressure to obtain an yttrium/aluminum-organic polymer precursor.
2. The method of preparing yttrium/aluminum-organic polymer precursor according to claim 1, wherein said aluminum source is one or a mixture of crystalline aluminum chloride and anhydrous aluminum chloride; the yttrium source is one or a mixture of crystalline yttrium chloride and anhydrous yttrium chloride; the organic solvent is absolute methanol, absolute ethanol or N, N-Dimethylformamide (DMF).
3. The method of claim 1, wherein the molar ratio of the aluminum source, yttrium source, acetylacetone, and triethylamine is 1: (0.5-0.7): (1.2-5.2): (2.4-9.6); the adding amount of the organic solvent is controlled to be 500-1000 g per 100 g of the aluminum source;
preferably, the mol ratio of the aluminum source to the yttrium source to the acetylacetone to the triethylamine is 1: 0.6: (1.28-3.2): (4-8);
preferably, the temperature of the reduced pressure drying is 30-40 ℃.
4. The method of claim 1, wherein the extractant is one or a mixture of acetone and tetrahydrofuran; the adding amount of the extracting agent is controlled to be 3000-3600 mL per mol of aluminum source, and the extracting time is 48-96 h.
5. An yttrium/aluminum-organic polymer precursor prepared according to any one of claims 1 to 4.
6. A method for preparing yttrium aluminum garnet continuous fibers comprising using the yttrium/aluminum-organic polymer precursor prepared according to claims 1 to 5, comprising the steps of:
dissolving an yttrium/aluminum-organic polymer precursor in an organic solvent, and obtaining precursor spinning sol after decompression and concentration; and preparing the precursor spinning sol into precursor continuous gel fiber through dry spinning, pretreating the precursor continuous gel fiber at 100-160 ℃, continuously heating to 800-1200 ℃ at the speed of 0.5-5 ℃/min, and preserving heat for 10-240 min to obtain the yttrium aluminum garnet continuous fiber.
7. The method of claim 6, wherein the yttrium/aluminum-organic polymer precursor and the organic solvent are present in a mass ratio of 1: (3-4);
preferably, the organic solvent is absolute methanol, absolute ethanol or N, N-Dimethylformamide (DMF);
preferably, the reduced pressure concentration temperature is 30-65 ℃, and the viscosity of the precursor spinning sol after reduced pressure concentration is 10-100 Pa.s at 20 ℃.
8. The method of claim 6, wherein the dry spinning process comprises: and (2) loading the precursor spinning sol into a liquid material tank of a spinning device, defoaming in vacuum for 1.5-2.5 h, pressurizing the precursor spinning sol by a steel cylinder nitrogen or metering pump at the temperature of 10-40 ℃ and the relative humidity of 20-80% to 0.5 MPa, ejecting the precursor spinning sol from a spinneret plate hole with the aperture of 0.04-0.20 mm, and performing multistage drafting and filament collection to obtain the precursor continuous gel fiber with the diameter of 30-150 mu m.
9. The method for preparing yttrium aluminum garnet continuous fiber according to claim 6, wherein the pretreatment is heat preservation in a steam environment of 120-140 ℃ for 10-30 min; the heating rate is 0.8-1.2 ℃/min, and the temperature is kept for 100-150 min; further preferably, the temperature rise rate is 1 ℃/min, and the temperature is kept for 120 min.
10. Yttrium aluminum garnet continuous fiber prepared according to any one of claims 6 to 9.
CN202010944335.4A 2020-09-10 2020-09-10 Yttrium/aluminum-organic polymer precursor, yttrium aluminum garnet continuous fiber and preparation method Pending CN111978550A (en)

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