CN107383376B - Method for preparing polyaluminum carbosilane precursor by taking aluminum stearate as aluminum source and application of polyaluminum carbosilane precursor - Google Patents

Method for preparing polyaluminum carbosilane precursor by taking aluminum stearate as aluminum source and application of polyaluminum carbosilane precursor Download PDF

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CN107383376B
CN107383376B CN201710569007.9A CN201710569007A CN107383376B CN 107383376 B CN107383376 B CN 107383376B CN 201710569007 A CN201710569007 A CN 201710569007A CN 107383376 B CN107383376 B CN 107383376B
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CN107383376A (en
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刘玉付
沈杰
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Southeast University
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
    • C—CHEMISTRY; METALLURGY
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    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/16—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/16—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/12—Applications used for fibers
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films

Abstract

The invention discloses a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source, which comprises the following steps: placing needed amount of polycarbosilane and aluminum stearate in a reaction vessel containing dimethylbenzene, and heating under stirring in an inert gas atmosphere until the mixed materials are completely dissolved in the dimethylbenzene; adjusting the temperature to 140-160 ℃ and reacting for 0.5-1 h; then adjusting the temperature to 220-350 ℃ and reacting for 1-5 h; and under the protection of inert atmosphere, reducing the reaction temperature to room temperature to prepare the polyaluminium carbosilane precursor. The invention also discloses application of the polyaluminum carbosilane precursor prepared by the method in preparing aluminum-containing silicon carbide fibers. The method for preparing the polyaluminum carbosilane precursor adopts aluminum stearate and polycarbosilane to synthesize the polyaluminum carbosilane precursor at high temperature and normal pressure, and aluminum stearate is not volatile easily in the synthesis process, so that the aluminum content in the aluminum-containing silicon carbide fiber can be effectively controlled.

Description

Method for preparing polyaluminum carbosilane precursor by taking aluminum stearate as aluminum source and application of polyaluminum carbosilane precursor
Technical Field
The invention relates to a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source, and also relates to application of the polyaluminum carbosilane precursor prepared by the method in the aspect of preparing aluminum-containing silicon carbide fibers, belonging to the technical field of inorganic fiber materials.
Technical Field
The silicon carbide (SiC) fiber is a high-performance ceramic fiber which is concerned by the material field in recent years, has the characteristics of small density, large specific strength, high specific modulus, small linear expansion coefficient, high temperature resistance, corrosion resistance, high strength and the like, has good composite compatibility with metal, ceramic, polymer and the like, and is an ideal reinforcing fiber of a high-performance composite material.
In order to improve the high temperature resistance of silicon carbide fibers, titanium-containing silicon carbide fibers, zirconium-containing silicon carbide fibers, boron-containing and nitrogen-containing silicon carbide fibers, aluminum-containing silicon carbide fibers, iron-containing silicon carbide fibers, nickel-containing silicon carbide fibers, niobium-containing silicon carbide fibers, cobalt-containing silicon carbide fibers and the like have been prepared at home and abroad by adding heterogeneous elements into the fibers. Among them, the aluminum-containing silicon carbide fiber is most excellent in high temperature resistance.
The effect of adding heterogeneous elements in the silicon carbide fiber is mainly as follows: (1) suppression of SiCxOyDecomposition of the phase, the heterogeneous elements often forming chemical bonds with oxygen, inhibiting SiC at high temperaturesxOyDecomposition of (2); (2) forming ultrahigh temperature carbide with C to improve the high temperature resistance of the fiber; (3) as a sintering aid, the heterogeneous element can effectively heal defects such as holes, cracks and the like in the silicon carbide fiber in the sintering process as the sintering aid, so that the density of the fiber is improved, and the strength is improved; (4) the growth of the SiC crystal is inhibited, and the growth of the crystal can be effectively inhibited because the coordination numbers of the heterogeneous elements and the SiC crystal are different.
The preparation method of the polyaluminum carbosilane (PACS) is mainly divided into two types, one type is the reaction of a solid organic silicon compound (solid polydimethylsilane, solid polycarbosilane, solid polysilane and the like) and an aluminum-containing compound (aluminum acetylacetonate, aluminum sec-butoxide and the like), and the preparation process has the defects that an aluminum element is difficult to enter the molecular structure of a polymer, an aluminum complex is easy to volatilize and lose, the system safety is lower, and the solvent is difficult to separate; the method has the advantages of no need of adding a solvent in the preparation process, no need of a circulating reflux process, simple and convenient method, high safety, short reaction time, low cost and the like, but has the possibility of uneven reaction (Li Yang. preparation and application research progress of polycarbosilane containing heterogeneous elements [ J ] novel chemical materials [ 2012, 40 (7): 148- & 151 ]).
Ishikawa et al, Japan, produced an aluminum-containing silicon carbide fiber TyrannosA (Ishikawa T, Kohtoku Y, Kumagawa K, et al, high-strength alkali-restrained SiC fiber stable to 2, 200 ℃ [ J ]. Nature.1998, 391: 773-phase 775) using PCS and aluminum acetylacetonate, and PACS was synthesized by heating PCS and aluminum acetylacetonate at 300 ℃ in a nitrogen atmosphere. The Tyranno SA silicon carbide fiber prepared by the method has the strength of more than 2.5GPa and the modulus of more than 300 GPa. The Tyranno SA fiber is subjected to heat treatment at 2000 ℃ for 1 hour under the argon atmosphere, and the strength retention rate is 80%. Heat treatment at 2200 ℃ in an inert gas atmosphere has very little mass loss. The Tyranno SA fiber has no strength reduction and no chemical composition change after being subjected to heat treatment at 1000 ℃ in an air atmosphere. Tyranno SA fibers also had very little creep at 1300 ℃. The Tyranno SA fiber can still maintain certain strength after being soaked in the salt solution and subjected to heat treatment in the air atmosphere.
The KD-SA type aluminum-containing silicon carbide fiber (Yuyu seal, continuous preparation and research of aluminum-containing silicon carbide fiber [ D ]. Changsha, space and material engineering college of the national defense science and technology university, 2005.) PACS precursor is synthesized by reacting poly-silicon carbosilane and aluminum acetylacetonate, the selection of the aluminum source is the same as that of Japan department of science and technology, and the difference is that PSCS is selected by the national defense science and technology university rather than PCS, because the national defense science and technology university finds that the aluminum acetylacetonate can be violently sublimated at about 150 ℃ when imitating the Japan department of science and technology to synthesize the aluminum-containing precursor by using PCS and aluminum acetylacetonate, the PCS cannot fully react with the aluminum acetylacetonate, and the PCS chooses to replace PCS by viscous PSCS. There is also a gap in the performance of KD-SA compared to Tyranno SA fibers from Japan. The tensile strength of the KD-SA fiber is 2.0-2.2GPa, and the elastic modulus is 370-410 GPa.
In addition, Chen Jiangxi of Xiamen university heats Polydimethylsiloxane (PDMS) and aluminum acetylacetonate in a high-pressure reaction kettle for reaction to prepare PACS (Chen Jiangxi, silicon carbide-based ceramic fiber, and the synthesis and characterization of organic silicon polymer [ D ]]A building door: chemical and chemical industry college of Xiamen university, 2007.) can effectively solve the problem of aluminum acetylacetonate sublimation by using a high-pressure reaction kettle. The presence of acetylacetone allows the formation of (Si-O) upon cleavage of PDMSnAl, thereby improving entanglement and having higher performance than PCS.
The Liquid Polycarbosilane (LPCS) for Yangjingming at the university of Xiamen is synthesized in a heating jacket of aluminum acetylacetonate, and a circulating reflux process is not carried out because the aluminum acetylacetonate does not volatilize in a large amount (Yangjingming, YangLujiao, Yuzui seal, and the like.
Li xudong et Al prepared PACS from Polysilane (PS) and aluminum acetylacetonate, formed Si-O bonds, Al-O bonds, and possibly Si-O-Al bonds. These chemical reactions form a network structure and thus the cleavage yield at 900 ℃ is greatly improved. When this precursor is cleaved under a nitrogen atmosphere at 1700 ℃ it is converted into a SiC-AlN ceramic (Li X D, Edisinghem J. structural introduction of Si-Al-C-O precursors and the iron pyrolysises products in nitrogen [ C ]. Proceedings of the Royal Society A: Physical, Physical and Engineering sciences.2003, 459 (2039): 2731-.
Babonneau et al prepared PACS precursor from PCS and aluminum sec-butoxide, dissolved in xylene, refluxed under argon atmosphere for 1 hour, distilled out the solvent, and heated to about 300 deg.C to obtain the crosslinked structure. Al (OH)3The structure exists in a PCS main chain through a Si-O-Al chemical bond, is converted into an inorganic substance at 800 ℃ during cracking, and consists of an amorphous phase, namely SiC, an aluminum-containing compound and carbon. At a temperature of more than 800 ℃, the aluminum-containing compound reacts with carbon to form Al-C bonds and Al2OC, and silicon carbide begins to crystallize into the 3C crystal form. At about 1300 deg.C, Al2OC reacts with SiC to generate SiC with 2H crystal form. At 1500 ℃, the main phases are SiC, SiC and Al in the 2H crystal form2OC and C react with each other to form a trace amount of Al4SiC4.(Babonneau F，Sorarú G D，Thorne K J，et al.Chemical characterization ofSi-Al-C-O precursor and its pyrolysis[J].Journal of the American CeramicSociety.1991，74(7)：1725-1728.)
In summary, the aluminum sources used for preparing the aluminum-containing silicon carbide fiber at home and abroad at present mainly comprise aluminum acetylacetonate, aluminum sec-butoxide and the like. Because the aluminum sources are easy to volatilize in the process of synthesizing the precursor, the content of aluminum in the aluminum-containing silicon carbide fiber is uncontrollable. If a high-pressure reaction kettle is adopted in the reaction process, the synthesis conditions are harsh.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source.
The invention also aims to solve the technical problem of providing the application of the polyaluminium carbosilane precursor prepared by the preparation method in the aspect of preparing the aluminium-containing silicon carbide fiber.
The polyaluminium carbosilane precursor prepared by the invention can be used for preparing aluminium-containing silicon carbide fibers, and can also be used for preparing films, coatings, matrixes of composite materials, high-temperature binders and the like.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source comprises the following steps:
step 1, putting required amount of PCS and aluminum stearate in a reaction vessel containing xylene, heating at 100 ℃ under an inert gas atmosphere and magnetically stirring until the mixed materials are completely dissolved in the xylene;
step 2, adjusting the reaction temperature of the mixed solution to 140-160 ℃ for reaction for 0.5-1 h;
step 3, adjusting the reaction temperature of the mixed solution to 220-350 ℃ and reacting for 1-5 h; the higher the temperature is, the longer the reaction time is, the higher the molecular weight of the precursor is, the poorer the spinning performance is, and the less the filament doubling is in the non-melting treatment and pyrolysis processes;
and 4, reducing the temperature from the reaction temperature in the step 3 to room temperature to prepare the polyaluminocarbosilane precursor.
Wherein in the step 1, the mass ratio of the PCS to the aluminum stearate is 30: 1-10: 1.
The polyaluminum carbosilane precursor prepared by the method for preparing the polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source is applied to the aspect of preparing aluminum-containing silicon carbide fibers.
The application of the polyaluminum carbosilane precursor prepared by the preparation method in the aspect of preparing the aluminum-containing silicon carbide fiber specifically comprises the following steps:
step 1, melting and spinning a polyaluminium carbosilane precursor to obtain a precursor;
step 2, the protofilament obtained in the step 1 is not melted for a period of time at a certain temperature;
step 3, pyrolyzing the precursor which is not subjected to melting treatment in the step 2 at 1000-1300 ℃ for 0.5-2 h to obtain the aluminum-containing silicon carbide fiber; the pyrolysis temperature is too low, the time is too short, the inorganic substances cannot be completely converted, the pyrolysis temperature is too high, the time is too long, crystal grains grow rapidly, and the fiber strength is reduced.
In the step 2, the air non-melting treatment temperature of the precursor is 160-220 ℃, the treatment time is 6-70 h, the higher the non-melting treatment temperature is, the less time is required, but the filament doubling can be realized at the non-melting treatment stage due to the overhigh temperature.
The protofilament is pyrolyzed for 0.5-2 hours in vacuum or inert atmosphere or hydrogen atmosphere, and the elemental composition proportion of the fiber can be changed by pyrolysis in different atmospheres, so that the performance of the fiber is changed.
Wherein the aluminum content of the prepared aluminum-containing silicon carbide fiber is 0.10-0.28 wt%, the diameter is less than or equal to 25 mu m, and the strength is not lower than 0.6 GPa.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
the preparation method of the polyaluminum carbosilane precursor adopts aluminum stearate and Polycarbosilane (PCS) to synthesize the polyaluminum carbosilane (PACS) precursor at high temperature and normal pressure, and aluminum stearate is not volatile in the synthesis process, so that the aluminum content in the aluminum-containing silicon carbide fiber can be effectively controlled; the preparation method has simple process flow, does not need a high-pressure reaction kettle, has mild reaction conditions, can effectively reduce the synthesis cost, has high product yield, and is suitable for industrial large-scale production; the finally prepared aluminum-containing silicon carbide fiber has excellent high temperature resistance and wide application prospect.
Drawings
FIG. 1 is a PACS precursor prepared in example 2 with a 10: 1 mass ratio of PCS to aluminum stearate;
FIG. 2 is a precursor spun-out strand of PACS prepared in example 1 with a 30: 1 mass ratio of PCS to aluminum stearate;
FIG. 3 is an FT-IR spectrum; wherein (c) corresponds to the FT-IR spectrum of the PACS precursor prepared by the mass ratio of PCS to aluminum stearate of 10: 1; (a) corresponding to FT-IR spectrum of PCS; (b) corresponding to the FT-IR spectrum of aluminum stearate; (d) corresponding to the FT-IR spectrum of xylene;
FIG. 4 is a partially enlarged FT-IR spectrum of FIG. 3; wherein (c) corresponds to the FT-IR spectrum of the PACS precursor prepared by the mass ratio of PCS to aluminum stearate of 10: 1; (a) corresponding to FT-IR spectrum of PCS; (b) corresponding to the FT-IR spectrum of aluminum stearate;
FIG. 5 is a surface topography of an aluminum-containing silicon carbide fiber of the present invention; wherein, (a) and (b) correspond to the aluminum-containing silicon carbide fiber prepared by the mass ratio of PCS to aluminum stearate of 30: 1; (c) and (d) corresponding to the aluminum-containing silicon carbide fiber prepared by the mass ratio of PCS to aluminum stearate of 10: 1;
FIG. 6 is a scanning electron microscopy spectroscopy analysis of aluminum-containing silicon carbide fibers of the present invention; wherein, (a) and (b) correspond to the aluminum-containing silicon carbide fiber prepared by the mass ratio of PCS to aluminum stearate of 30: 1; (c) and (d) corresponding to the aluminum-containing silicon carbide fiber prepared by the mass ratio of PCS to aluminum stearate of 10: 1.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the specific embodiments, but the scope of the present invention is not limited thereto.
Example 1
The invention discloses a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source, which comprises the following steps: adding 30 parts by mass of PCS and 1 part by mass of aluminum stearate into a three-neck flask filled with xylene, heating to 100 ℃, and magnetically stirring to completely dissolve the PCS and the aluminum stearate in the xylene; heating to 160 ℃, and preserving heat for 0.5h to remove part of xylene in the reaction material; and continuously heating to 350 ℃, preserving the temperature for 1h, removing all dimethylbenzene in the reaction materials, simultaneously fully reacting and crosslinking aluminum stearate and PCS to obtain a polyaluminium carbosilane precursor, cooling the temperature to room temperature, and carrying out the whole process of synthesizing the polyaluminium carbosilane precursor in an inert atmosphere.
The application of the polyaluminum carbosilane precursor prepared by the preparation method in the aspect of preparing the aluminum-containing silicon carbide fiber is as follows: melt spinning the prepared polyaluminium carbosilane precursor to obtain precursor; carrying out non-melting treatment on the obtained protofilament in air at 180 ℃ for 15 h; and (3) carrying out vacuum pyrolysis on the protofilament which is not subjected to melting treatment at 1000 ℃ for 0.5h to obtain the needed aluminum-containing silicon carbide fiber. The theoretical aluminium content of the fibre produced is 0.10 wt%, the diameter is 15 μm, and the average strength is 1.0 GPa.
Example 2
The invention discloses a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source, which comprises the following steps: adding 30 parts by mass of PCS and 3 parts by mass of aluminum stearate into a three-neck flask filled with xylene, heating to 100 ℃, and magnetically stirring to completely dissolve the PCS and the aluminum stearate in the xylene; heating to 140 ℃, and preserving heat for 1h to remove part of xylene in the reaction material; and continuously heating to 300 ℃, preserving the temperature for 3h, removing all dimethylbenzene in the reaction materials, simultaneously fully reacting and crosslinking aluminum stearate and PCS to obtain a polyaluminium carbosilane precursor, cooling the temperature to room temperature, and synthesizing the polyaluminium carbosilane precursor under an inert atmosphere.
The application of the polyaluminum carbosilane precursor prepared by the preparation method in the aspect of preparing the aluminum-containing silicon carbide fiber is as follows: melt spinning the prepared polyaluminium carbosilane precursor to obtain precursor; carrying out non-melting treatment on the obtained protofilament in air at 220 ℃ for 6 h; and pyrolyzing the protofilament which is not subjected to melting treatment in a hydrogen atmosphere at 1300 ℃ for 2h to obtain the required aluminum-containing silicon carbide fiber. The resulting fiber had a theoretical aluminum content of 0.28 wt%, a diameter of 25 μm and an average strength of 0.6 GPa.
Example 3
The invention discloses a method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source, which comprises the following steps: adding 15 parts by mass of PCS and 1 part by mass of aluminum stearate into a three-neck flask filled with xylene, heating to 100 ℃, and magnetically stirring to completely dissolve the PCS and the aluminum stearate in the xylene; heating to 150 ℃, and preserving the temperature for 1h to remove part of dimethylbenzene in the reaction material; and continuously heating to 220 ℃, preserving the temperature for 5h, removing all dimethylbenzene in the reaction materials, simultaneously fully reacting and crosslinking aluminum stearate and PCS to obtain a polyaluminium carbosilane precursor, cooling the temperature to room temperature, and synthesizing the polyaluminium carbosilane precursor under an inert atmosphere.
The application of the polyaluminum carbosilane precursor prepared by the preparation method in the aspect of preparing the aluminum-containing silicon carbide fiber is as follows: melt spinning the prepared polyaluminium carbosilane precursor to obtain precursor; carrying out non-melting treatment on the obtained protofilament for 70 hours at 160 ℃ in the air; and pyrolyzing the protofilament which is not subjected to melting treatment in an argon atmosphere at 1200 ℃ for 1h to obtain the required aluminum-containing silicon carbide fiber. The theoretical aluminium content of the fibre produced is 0.19 wt%, the diameter is 12 μm and the average strength is 1.2 GPa.
FIG. 4 is a partially enlarged FT-IR spectrum of FIG. 3, and 2851cm was found in the synthesized precursor (c)-1And 2923cm-1Two peaks, are CH2The C-H stretching vibrational peak in the structure, which is absent in PCS (a) and likewise absent in aluminum stearate (b), indicates that aluminum stearate chemically reacted with PCS.
FIG. 5 is a surface topography of an aluminum-containing silicon carbide fiber of the present invention; as can be seen from fig. 5, the diameter of the same batch of fibers is uniform, and the surface defects such as holes, cracks, grooves and the like are not obvious on the surface of the fibers.
FIG. 6 is a scanning electron microscopy spectroscopy analysis of aluminum-containing silicon carbide fibers of the present invention; as can be seen from fig. 6, the aluminum-containing silicon carbide fiber obtained had aluminum elements detected in addition to the main C, Si, O elements and H elements that could not be detected.
It should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And such obvious variations or modifications which fall within the spirit of the invention are intended to be covered by the scope of the present invention.

Claims (2)

1. A method for preparing a polyaluminum carbosilane precursor by taking aluminum stearate as an aluminum source is characterized by comprising the following steps: the method comprises the following steps:
step 1, putting required amount of PCS and aluminum stearate in a reaction vessel containing xylene, heating at 100 ℃ under an inert gas atmosphere and magnetically stirring until the mixed materials are completely dissolved in the xylene;
step 2, adjusting the reaction temperature of the mixed solution to 140-160 ℃ for reaction for 0.5-1 h;
step 3, adjusting the reaction temperature of the mixed solution to 220-350 ℃ and reacting for 1-5 h;
and 4, reducing the temperature from the reaction temperature in the step 3 to room temperature to prepare the polyaluminocarbosilane precursor.
2. The method of claim 1 for preparing a polyaluminum carbosilane precursor with aluminum stearate as aluminum source, wherein: in the step 1, the mass ratio of the PCS to the aluminum stearate is 30: 1-10: 1.
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