CN114409420B - Alumina fiber reinforced mullite ceramic matrix composite and preparation method thereof - Google Patents
Alumina fiber reinforced mullite ceramic matrix composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an alumina fiber reinforced mullite ceramic matrix composite and a preparation method thereof, relating to the technical field of fiber reinforced ceramic composites, wherein the preparation method comprises the following steps: preparing mullite slurry by ball milling, pretreating alumina fiber cloth, preparing a lanthanum phosphate interface layer, carrying out vacuum-hot press molding and densification to finally obtain an alumina fiber reinforced mullite ceramic matrix composite finished product. The invention adopts alumina fiber as the reinforcing phase to reinforce the strength of the alumina matrix, the preparation process is simple, and the prepared finished product has excellent high-temperature mechanical properties.
Description
Technical Field
The invention relates to the technical field of fiber reinforced ceramic composite materials, in particular to an alumina fiber reinforced mullite ceramic matrix composite material and a preparation method thereof.
Background
The continuous alumina fiber reinforced mullite ceramic matrix composite has high temperature resistance, oxidation resistance, good mechanical property strength and heat insulation property, can be used for a long time under a high temperature condition, and has wide application prospects in the fields of aviation, aerospace, nuclear energy and the like. The vacuum impregnation-drying-heat treatment forming process of the three-dimensional fabric weaves alumina fiber into a fiber preform, and then impregnation-drying is carried out. The method comprises the steps of pretreating the fabric to remove the sizing agent, then carrying out repeated impregnation-drying densification treatment by using an organic precursor solution or sol as a matrix, and finally carrying out heat treatment to obtain the alumina fiber reinforced ceramic matrix composite. Chinese patent publication Nos. CN105254320A, CN106699209A and CN106966742A respectively disclose an oxide fiber reinforced ceramic matrix composite based on an impregnation-curing-heat treatment process and a preparation method thereof. This method has some disadvantages: firstly, because the ceramic yield of the organic precursor or the sol is low and generally does not exceed 20wt%, the ceramic needs to be repeatedly dipped and subjected to high-temperature heat treatment for more than 10 times, and the thermal damage of the alumina fiber is easily aggravated by multiple heat treatments, so that the mechanical property of the composite material is reduced. Secondly, the process has long period, low efficiency and high process cost.
Chinese patent publication No. CN110590388a discloses a prepreg-hot press molding method of alumina fiber reinforced alumina ceramic. The method adopts the alumina powder ball-milling slurry as a matrix, can realize the rapid preparation of the composite material, and has simple process and low cost. But the sintering activity of the alumina powder is low, and the combination among particles is weak; in addition, the fiber is easy to react with the matrix under high temperature without the protection of the interface layer, so that the performance of the composite material is reduced.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention aims to provide the alumina fiber reinforced mullite ceramic matrix composite and the preparation method thereof, wherein the alumina fiber is used as a reinforcing phase to reinforce the strength of an alumina matrix.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of an alumina fiber reinforced mullite ceramic matrix composite material comprises the following steps:
1) Preparing mullite slurry by ball milling: mixing mullite powder, mullite sol and citric acid, and then carrying out ball milling to obtain mullite slurry;
2) Pretreatment of the alumina fiber cloth: arranging the alumina fiber in a muffle furnace for heating treatment to obtain an alumina fiber preform, removing the impregnating compound on the surface of the alumina fiber preform, naturally cooling, and taking out to obtain a continuous alumina fiber preform without the impregnating compound;
3) Preparing a lanthanum phosphate interface layer: preparing a lanthanum phosphate precursor solution, dipping the continuous alumina fiber preform into the lanthanum phosphate precursor solution for reaction, then taking the continuous alumina fiber preform out of the lanthanum phosphate precursor solution, cleaning the continuous alumina fiber preform for a plurality of times by using ultrapure water, then placing the continuous alumina fiber preform into an oven for drying, and then carrying out heat treatment in a muffle furnace to obtain alumina fiber cloth containing a lanthanum phosphate interface layer;
4) Vacuum-hot press molding: arranging the alumina fiber containing the lanthanum phosphate interface layer in a mold, coating mullite slurry on the surface of the alumina fiber cloth containing the lanthanum phosphate interface layer, layering layer by layer, coating the mullite slurry layer by layer, and placing in a vacuum press for vacuum-hot press molding after layering is finished to obtain an alumina fiber reinforced mullite ceramic matrix composite blank;
5) Densification: and placing the alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum tank, dipping the mullite sol, then placing the blank in a vacuum oven for drying, placing the dried blank in a muffle furnace for heat treatment, and circularly carrying out dipping, drying and heat treatment for 4-6 times until the composite material is not weighted any more, thereby obtaining the alumina fiber reinforced mullite ceramic matrix composite finished product.
Further, the mass ratio of the mullite powder to the mullite sol to the citric acid in the step 1) is (40-100) to (100-200) to (1-3).
Further, the ceramic yield of the mullite sol in the step 1) is 10-20 wt%.
Further, the ceramic yield of the mullite slurry in the step 1) is 20 to 60wt%, preferably 40wt%.
Further, the alumina fiber cloth in the step 2) is satin cloth, twill cloth or plain cloth made of alumina fibers.
Further, the heating treatment temperature in the step 2) is 500-600 ℃, and the heating treatment time is 1-3 h.
Further, the reaction temperature of the solution for dipping the continuous alumina fiber preform into the lanthanum phosphate precursor in the step 3) is 50-70 ℃, and the reaction time is 1-2 h; the drying temperature in the oven is 80-120 ℃, and the drying time is 12-24 h; the heat treatment temperature in a muffle furnace is 800-1000 ℃, and the heat treatment time is 1-2 h.
Further, the hot pressing temperature of the vacuum-hot pressing molding in the step 4) is 120-300 ℃, and the hot pressing time is 2-6h, preferably 180 ℃ and 4h.
Further, in the step 5), the drying temperature is 40-80 ℃, and the drying time is 18-36h, preferably 60 ℃ and 24h.
Further, the heat treatment temperature in the step 5) is 1000-1200 ℃, and the heat treatment time is 1-4h, preferably 1100 ℃ and 2h.
An alumina fiber reinforced mullite ceramic matrix composite is prepared by the method.
The invention achieves the following beneficial effects: firstly, the alumina fiber reinforced mullite ceramic matrix composite provided by the invention is prepared by preparing a lanthanum phosphate interface layer on the surface of alumina fiber, and can effectively improve the strong bonding between the fiber and a matrix. Secondly, mullite powder and mullite sol are mixed and ball-milled to prepare mullite slurry, the mullite powder particles with low sintering activity are used as filler, the mullite sol particles with high sintering activity are used as binder, and the sintering activity of the matrix can be maintained while the impregnation efficiency is improved. Finally, the composite material provided by the invention has excellent high-temperature mechanical properties, and the preparation method is simple and feasible, low in cost and short in period.
Drawings
FIG. 1 is a flow chart of a method for preparing an alumina fiber reinforced mullite ceramic matrix composite provided by the present invention.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
S1, preparing mullite slurry: adding mullite powder, mullite sol and citric acid into a ball milling tank, adding large and small grinding balls, setting the rotating speed of a ball mill to be 150rpm, and carrying out ball milling for 8 hours to obtain mullite slurry with the ceramic yield of 20wt%. Wherein the mass ratio of the mullite powder to the mullite sol to the citric acid is 40.
S2, pretreatment of the alumina fiber preform: and (3) placing the aluminum oxide fiber satin cloth in a muffle furnace, heating to 500 ℃, preserving heat for 3 hours, and naturally cooling to room temperature to obtain the aluminum oxide fiber preform without the impregnating compound.
S3, preparing a lanthanum phosphate interface layer: preparing a lanthanum phosphate precursor solution by adopting the existing preparation method such as CN110983757A, and stirring and mixing a lanthanum nitrate solution (0.4 mol/L) and a phosphoric acid solution (0.4 mol/L) at 1 ℃ to obtain a lanthanum phosphate precursor solution; dipping the alumina fiber preform without the wetting agent into a lanthanum phosphate precursor solution, reacting for 1h at 70 ℃, taking out the alumina fiber preform from the lanthanum phosphate precursor solution, cleaning the alumina fiber preform with ultrapure water for three times, drying the alumina fiber preform in an oven at 80 ℃ for 24h, and performing heat treatment in a muffle furnace at 900 ℃ for 1.5h to obtain alumina fiber cloth containing a lanthanum phosphate interface layer;
s4, vacuum-hot press molding: arranging alumina fibers containing a lanthanum phosphate interface layer in a mold, coating mullite slurry on the surface of the alumina fiber cloth containing the lanthanum phosphate interface layer, continuously layering layer by layer and coating the mullite slurry, and after layering is finished, arranging the alumina fiber cloth in a vacuum press for vacuum-hot press molding at the hot pressing temperature of 120 ℃ for 6 hours to obtain an alumina fiber reinforced mullite ceramic matrix composite blank;
s5, densification: placing the alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum tank, soaking the mullite sol, then placing the impregnated alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum oven for drying at 40 ℃, preserving heat for 36 hours, finally placing the impregnated alumina fiber reinforced mullite ceramic matrix composite blank in a muffle furnace for heat treatment at 1000 ℃ for 3 hours, and carrying out 4 times of cyclic soaking-drying-heat treatment to obtain the alumina fiber reinforced mullite ceramic matrix composite finished product.
Example 2
S1, preparing mullite slurry: adding mullite powder, mullite sol and citric acid into a ball milling tank, adding large and small grinding balls, setting the rotating speed of a ball mill to 300rpm, and carrying out ball milling for 8 hours to obtain mullite slurry with the ceramic yield of 40wt%. Wherein the mass ratio of the mullite powder to the mullite sol to the citric acid is 80.
S2, pretreatment of the alumina fiber preform: and placing the alumina fiber twill cloth in a muffle furnace, heating to 600 ℃, preserving heat for 1h, and naturally cooling to room temperature to obtain the alumina fiber preform without the impregnating compound.
S3, preparing a lanthanum phosphate interface layer: stirring and mixing a lanthanum nitrate solution (0.6 mol/L) and a phosphoric acid solution (0.6 mol/L) at the temperature of 2 ℃ to obtain a lanthanum phosphate precursor solution; dipping the alumina fiber preform without the wetting agent into a lanthanum phosphate precursor solution, reacting for 2h at 50 ℃, taking out the alumina fiber preform from the lanthanum phosphate precursor solution, cleaning the alumina fiber preform with ultrapure water for three times, placing the alumina fiber preform in a drying oven, drying for 12h at 120 ℃, and performing heat treatment for 1h at 1000 ℃ in a muffle furnace to obtain alumina fiber cloth containing a lanthanum phosphate interface layer;
s4, vacuum-hot press molding: arranging alumina fibers containing a lanthanum phosphate interface layer in a mold, coating mullite slurry on the surface of the alumina fiber cloth containing the lanthanum phosphate interface layer, continuously layering layer by layer and coating the mullite slurry, and after layering is finished, placing the alumina fiber cloth in a vacuum press for vacuum-hot press molding at the hot pressing temperature of 300 ℃ for 2 hours to obtain an alumina fiber reinforced mullite ceramic matrix composite blank;
s5, densification: placing the alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum tank, soaking mullite sol, then placing in a vacuum oven for drying at 60 ℃, preserving heat for 24 hours, finally placing in a muffle furnace for heat treatment at 1200 ℃, preserving heat for 1 hour, and carrying out 6 times of cyclic soaking-drying-heat treatment to obtain the alumina fiber reinforced mullite ceramic matrix composite finished product.
Example 3
S1, preparing mullite slurry: adding mullite powder, mullite sol and citric acid into a ball milling tank, adding large and small grinding balls, setting the rotating speed of the ball mill at 500rpm, and carrying out ball milling for 8 hours to obtain the mullite slurry with the ceramic yield of 60wt%. Wherein the mass ratio of the mullite powder to the mullite sol to the citric acid is 100.
S2, pretreatment of the alumina fiber preform: and (3) placing the alumina fiber plain cloth in a muffle furnace, heating to 550 ℃, preserving heat for 1.5h, and naturally cooling to room temperature to obtain the alumina fiber preform without the impregnating compound.
S3, preparing a lanthanum phosphate interface layer: stirring and mixing a lanthanum nitrate solution (0.5 mol/L) and a phosphoric acid solution (0.5 mol/L) at 1 ℃ to obtain a lanthanum phosphate precursor solution; dipping the alumina fiber preform without the impregnating compound in a lanthanum phosphate precursor solution, reacting for 1.5h at 60 ℃, taking out the alumina fiber preform from the lanthanum phosphate precursor solution, cleaning the alumina fiber preform with ultrapure water for three times, drying the alumina fiber preform in an oven at 100 ℃ for 18h, and performing heat treatment in a muffle furnace at 800 ℃ for 2h to obtain alumina fiber cloth containing a lanthanum phosphate interface layer;
s4, vacuum-hot press molding: arranging alumina fibers containing a lanthanum phosphate interface layer in a mold, coating mullite slurry on the surface of the alumina fiber cloth containing the lanthanum phosphate interface layer, continuously layering layer by layer and coating the mullite slurry, and after layering is finished, placing the alumina fiber cloth in a vacuum press for vacuum-hot press molding at the hot pressing temperature of 180 ℃ for 4 hours to obtain an alumina fiber reinforced mullite ceramic matrix composite blank;
s5, densification: placing the alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum tank, soaking mullite sol, then placing in a vacuum oven for drying at 80 ℃, preserving heat for 18h, finally placing in a muffle furnace for heat treatment at 1100 ℃ for 2h, and carrying out 5 times of cyclic soaking-drying-heat treatment to obtain the alumina fiber reinforced mullite ceramic matrix composite finished product.
Referring to the process parameter conditions of example 3, mullite slurry was prepared by ball milling of mullite powder and citric acid (without mullite sol), and the alumina fiber reinforced mullite ceramic matrix composite containing a lanthanum phosphate interface layer was prepared as comparative example 1; referring to the process parameter conditions of example 3, an alumina fiber reinforced mullite ceramic matrix composite without a lanthanum phosphate interfacial layer was prepared as comparative example 2. And (3) comparing the mechanical property test of the alumina fiber reinforced mullite ceramic matrix composite obtained in the example 3 with the samples obtained in the comparative examples 1-2 to obtain the main performance parameters shown in the table 1. As can be seen from Table 1, the alumina fiber reinforced mullite ceramic matrix composite prepared in example 3 has excellent high-temperature mechanical properties; in contrast, the mullite sol is not added in the comparative example 1, and the lanthanum phosphate interface layer is not contained in the comparative example 2, so that the prepared alumina fiber reinforced mullite ceramic matrix composite material has poor tensile and compressive strength properties.
TABLE 1 alumina fiber reinforced mullite ceramic matrix composite finished product Performance parameters
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The preparation method of the alumina fiber reinforced mullite ceramic matrix composite is characterized by comprising the following steps:
1) Mixing mullite powder, mullite sol and citric acid, and then carrying out ball milling to obtain mullite slurry;
2) Arranging the alumina fiber in a muffle furnace for heating treatment at the temperature of 500-600 ℃ for 1-3 h to obtain an alumina fiber preform, removing the impregnating compound on the surface of the alumina fiber preform, naturally cooling, and taking out to obtain a continuous alumina fiber preform without the impregnating compound;
3) Preparing a lanthanum phosphate precursor solution, dipping the continuous alumina fiber preform into the lanthanum phosphate precursor solution for reaction, then taking the continuous alumina fiber preform out of the lanthanum phosphate precursor solution, cleaning the continuous alumina fiber preform for a plurality of times by using ultrapure water, then placing the continuous alumina fiber preform into an oven for drying, and then carrying out heat treatment in a muffle furnace to obtain alumina fiber cloth containing a lanthanum phosphate interface layer;
4) Arranging the alumina fiber containing the lanthanum phosphate interface layer in a mold, coating mullite slurry on the surface of the alumina fiber cloth containing the lanthanum phosphate interface layer, layering layer by layer, coating the mullite slurry layer by layer, and placing in a vacuum press for vacuum-hot press molding after layering is finished to obtain an alumina fiber reinforced mullite ceramic matrix composite blank;
5) And placing the alumina fiber reinforced mullite ceramic matrix composite blank in a vacuum tank, dipping the mullite sol, then placing the blank in a vacuum oven for drying, placing the dried blank in a muffle furnace for heat treatment, and circularly carrying out dipping, drying and heat treatment for 4-6 times until the composite material is not weighted any more, thereby obtaining the alumina fiber reinforced mullite ceramic matrix composite finished product.
2. The method of claim 1, wherein the mass ratio of the mullite powder, the mullite sol and the citric acid in the step 1) is (40-100) to (100-200) to (1-3).
3. The method of claim 1, wherein the ceramic yield of the mullite sol in step 1) is 10 to 20 weight percent; the ceramic yield of the mullite slurry is 20-60 wt%.
4. The method of claim 1, wherein the alumina fiber cloth in the step 2) is a satin, twill or plain cloth made of alumina fibers.
5. The method according to claim 1, wherein the reaction temperature for impregnating the continuous alumina fiber preform with the lanthanum phosphate precursor solution in step 3) is 50-70 ℃ and the reaction time is 1-2 h; the drying temperature in the oven is 80-120 ℃, and the drying time is 12-24 h; the heat treatment temperature in a muffle furnace is 800-1000 ℃, and the heat treatment time is 1-2 h.
6. The method of claim 1, wherein the hot pressing temperature of the vacuum-hot press molding in the step 4) is 120 to 300 ℃ and the hot pressing time is 2 to 6 hours.
7. The method of claim 1, wherein the drying temperature in step 5) is 40-80 ℃ and the drying time is 18-36h.
8. The method according to claim 1, wherein the heat treatment temperature in step 5) is 1000 to 1200 ℃ and the heat treatment time is 1 to 4 hours.
9. An alumina fiber reinforced mullite ceramic matrix composite produced by the method of any one of claims 1-8.
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| CN115043665A (en) * | 2022-06-07 | 2022-09-13 | 哈尔滨工业大学 | Porous mullite-lanthanum phosphate complex phase wave-transmitting material and preparation method thereof |
| CN115417683A (en) * | 2022-07-11 | 2022-12-02 | 东华大学 | Preparation method of oxide continuous filament reinforced oxide ceramic matrix composite |
| CN115182074B (en) * | 2022-07-15 | 2024-01-30 | 中南大学 | Rare earth lanthanum oxide modified alumina-mullite fiber and preparation method thereof |
| CN115124361B (en) * | 2022-07-15 | 2023-03-03 | 南通大学 | Ceramic matrix composite material with hybrid structure and preparation method thereof |
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| CN115974536B (en) * | 2023-01-17 | 2024-02-13 | 航天特种材料及工艺技术研究所 | Alumina fiber reinforced ceramic matrix composite containing lanthanum phosphate interface layer and preparation method thereof |
| CN116332665A (en) * | 2023-03-08 | 2023-06-27 | 航天特种材料及工艺技术研究所 | Preparation method of alumina fiber reinforced alumina ceramic matrix composite material containing low-mode interface |
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