CN105272325B - Preparation method of continuous oxide fiber fabric surface coating - Google Patents
Preparation method of continuous oxide fiber fabric surface coating Download PDFInfo
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- CN105272325B CN105272325B CN201510779681.0A CN201510779681A CN105272325B CN 105272325 B CN105272325 B CN 105272325B CN 201510779681 A CN201510779681 A CN 201510779681A CN 105272325 B CN105272325 B CN 105272325B
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Abstract
The invention belongs to a preparation technology of a continuous fiber reinforced ceramic matrix composite, and relates to a preparation method of a coating interface between fibers and a matrix in a continuous oxide fiber reinforced oxide ceramic matrix composite. Firstly, preparing a coating phase phosphate precursor solution, then dipping an oxide fiber preform into the precursor solution, taking out the preform after the dipping is finished, carrying out desizing treatment at a proper temperature, and obtaining a phosphate coating on the surface of the fiber through a repeated dipping-heat treatment process. The coating not only can protect the fiber from mechanical and thermal damage in the densification process of the matrix, but also can provide a proper weak interface combination for the fiber and the matrix, thereby improving the strength and the toughness of the material. In addition, the phosphate coating has the characteristic of high-temperature oxidation resistance, so that the service life and the high-temperature reliability of the composite material can be greatly improved.
Description
Technical Field
The invention belongs to a preparation technology of a continuous fiber reinforced ceramic matrix composite, and relates to a preparation method of a continuous oxide fiber fabric surface coating.
Background
The continuous fiber reinforced composite material has the characteristics of low density, high specific strength, high specific modulus, high temperature resistance, oxidation resistance, good reliability and the like, and is the development direction of high-performance aeroengine materials. The Ceramic Matrix Composite (CMC) is a structural material with high use temperature (1650 ℃) and low density (2.5g/cm 3-3.3 g/cm3), and is expected to replace nickel base or single crystal nickel alloy with the density of more than 8.0g/cm3 to be used as components of a combustion chamber, a flame stabilizer, an inner cone, a tail nozzle, a worm gear outer ring, a high-pressure turbine, a low-pressure turbine and the like of an engine. Compared with the SiCf/SiC composite material successfully proved by demonstration on the aeroengine, the oxide fiber reinforced oxide ceramic matrix composite material has better oxidation resistance and lower cost, and is likely to be used in a gas environment mirror at 1000-1300 ℃ for a long time.
The fiber, the matrix and the interface are three major elements of the fiber reinforced composite material, in the fiber reinforced ceramic matrix composite material, the interface layer is a tie connecting the reinforcing phase fiber and the continuous phase matrix, and the components and the structure of the interface layer determine the bonding strength between the fiber and the matrix and determine the toughening effect. The fracture behavior of the fiber reinforced ceramic matrix composite under the action of external load mainly comprises the forms of crack deflection, microcrack formation, interface dissociation, fiber fracture, fiber extraction and the like, wherein the fiber extraction is the most important energy release path, and the interface dissociation is a precondition for the extraction of the fibers from a matrix. If the interface bonding force is strong, the ceramic fiber is difficult to achieve the toughening effect, so that the material is subjected to brittle fracture under the impact of external load; if the interface bonding strength is too low, the matrix cannot transmit external load to the ceramic fibers through the interface, and the reinforcement effect is difficult to achieve. Therefore, the interfacial layer is one of the direct and critical factors affecting the mechanical properties of the ceramic matrix composite, and must be strictly designed and controlled in the preparation process.
At present, the interface layer of the fiber reinforced ceramic matrix composite mainly comprises a pyrolytic carbon interface layer and a BN interface layer, but the pyrolytic carbon and BN interface mainly aims at the non-oxide continuous fiber reinforced ceramic matrix composite, and because the oxide fiber reinforced oxide ceramic matrix composite is mainly used in oxygen and gas environments, service conditions are harsh, and the pyrolytic carbon and BN interface can not meet the requirements of oxidation resistance, long service life and high reliability in the service environment.
Disclosure of Invention
The purpose of the invention is: provides a preparation method of a phosphate coating on the surface of high-temperature-resistant and oxidation-resistant oxide fiber.
The technical scheme of the invention is as follows: the method comprises the following operation steps:
(6) pretreatment of continuous fiber preforms
Removing the sizing agent on the surface of the continuous fiber preform by a physical mode of high-temperature heat treatment or a chemical mode of solvent dissolution for later use;
(7) preparation of coating phase precursor solution
Preparing a coating precursor solution by a solution stirring and mixing mode, wherein the precursor solution is one or more of the following mixed solutions, namely a mixed solution of nitrate and phytic acid, a mixed solution of nitrate and phosphoric acid, a mixed solution of citric acid and a mixed solution of nitrate and ammonium dihydrogen phosphate, and the concentration of the nitrate in the coating precursor solution is 30-80%;
(8) continuous oxide fiber preform impregnation process
Immersing the pretreated continuous oxide fiber preform into the precursor solution for 10-20s, taking out, putting into deionized water at 50-100 ℃, continuously stirring for 5-15min, and washing the surface of the fiber cloth by the deionized water after taking out so as to remove ions in the solution and loose solids on the surface;
(9) drying and heat treatment process of coating
Drying the fiber preform impregnated with the precursor solution in an oven, and then placing the fiber preform in a muffle furnace for heat treatment, wherein the fiber preform impregnated with the precursor solution is dried in the oven at the drying temperature of 80-150 ℃ for 10-20min, the heat treatment temperature is 500-1100 ℃ and the heat treatment time is 3-10 min;
(10) control of coating thickness
And (4) repeatedly carrying out the steps (3) and (4) on the fiber preform after the heat treatment until a desired coating thickness is obtained.
The invention has the advantages and beneficial effects that:
firstly, the phosphate coating prepared by the invention has low bonding strength with most oxides, is nontoxic, insoluble in water, acid and alkali solutions, has high melting point and good high-temperature stability (>1400 ℃), has low hardness (5GPa), is easy to form plastic deformation when a fiber-matrix slips, and is an ideal coating material for oxide fibers.
Secondly, the phosphate coating interface prepared by the invention plays a role in protecting the fiber from being thermally damaged by a matrix precursor solution and a heat treatment process in a matrix densification process, and meanwhile, the monazite structure of the phosphate forms a weak interface between the fiber and the matrix, so that the strength and the toughness of the composite material are improved to the maximum extent. In addition, the oxidation resistance of the phosphate greatly improves the life and reliability of the composite material.
Thirdly, the equipment of the invention has low requirement, does not need CVD equipment used in the preparation process of the cracked carbon and BN interface, does not need atmosphere protection, can be finished in the air atmosphere, has short preparation period, and can realize the preparation of ideal coating thickness within 2-3 hours.
Fourthly, the raw materials adopted by the invention have wide sources, low cost, simple operation, safety and easy operation.
Fifthly, the interface coating prepared by the invention can control the structure and thickness of the coating through the dipping time and times of the fiber in the precursor solution, the structural design is flexible and controllable, and the interface coating can be designed according to different use requirements and matrix characteristics.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The method comprises the following operation steps:
(11) pretreatment of continuous fiber preforms
Removing the sizing agent on the surface of the continuous fiber preform by a physical mode of high-temperature heat treatment or a chemical mode of solvent dissolution for later use;
(12) preparation of coating phase precursor solution
Preparing a coating precursor solution by a solution stirring and mixing mode, wherein the precursor solution is one or more of the following mixed solutions, namely a mixed solution of nitrate and phytic acid, a mixed solution of nitrate and phosphoric acid, a mixed solution of citric acid and a mixed solution of nitrate and ammonium dihydrogen phosphate, and the concentration of the nitrate in the coating precursor solution is 30-80%;
(13) continuous oxide fiber preform impregnation process
Immersing the pretreated continuous oxide fiber preform into the precursor solution for 10-20s, taking out, putting into deionized water at 50-100 ℃, continuously stirring for 5-15min, and washing the surface of the fiber cloth by the deionized water after taking out so as to remove ions in the solution and loose solids on the surface;
(14) drying and heat treatment process of coating
Drying the fiber preform impregnated with the precursor solution in an oven, and then placing the fiber preform in a muffle furnace for heat treatment, wherein the fiber preform impregnated with the precursor solution is dried in the oven at the drying temperature of 80-150 ℃ for 10-20min, the heat treatment temperature is 500-1100 ℃ and the heat treatment time is 3-10 min;
(15) control of coating thickness
And (4) repeatedly carrying out the steps (3) and (4) on the fiber preform after the heat treatment until a desired coating thickness is obtained.
Example 1
Placing the alumina fiber fabric of which the model is 610 and which is manufactured by 3M company in a muffle furnace for heat treatment at 800 ℃ for 1h, and removing the surface sizing agent for later use.
Lanthanum nitrate (La (NO3) 3.6H 2O) and phytic acid (pc) are stirred and mixed in deionized water to prepare a precursor solution, wherein the concentration of the lanthanum nitrate is 50%. Then, the alumina fiber fabric is immersed in the precursor solution for 15s and then taken out, the alumina fiber fabric is taken out and then put into deionized water at 90 ℃, the deionized water is continuously stirred for 5min, LaPO4 is deposited on the surface of the fiber fabric, and the surface of the fiber fabric with the coating is washed by the deionized water for 20s after the alumina fiber fabric is taken out, so that ions in the solution and loose solids on the surface are removed. And then, drying the fiber in an oven at 120 ℃ for 15min, then placing the fiber in a muffle furnace, carrying out heat treatment at 800 ℃ for 5min, directly taking out the fiber, and carrying out immersion-heat treatment cycle for 6 times in such a way, and finally preparing a LaPO4 interface phase on the surface of the fiber woven fabric. The final thickness of the interface phase is 210-250nm through weight gain calculation.
Example 2
Soaking mullite fiber fabric produced by Mitsubishi company of Japan in acetone for 30min, placing in a muffle furnace for heat treatment at 500 ℃ for 2h, and removing surface sizing agent for later use.
Neodymium nitrate (Nd (NO3) 3.6H 2O) and Ammonium Dihydrogen Phosphate (ADPH) are magnetically stirred and mixed in deionization to prepare a precursor solution, wherein the concentration of lanthanum nitrate is 60%. Then, the alumina fiber fabric is immersed in the precursor solution for 10s and then taken out, the alumina fiber fabric is put into deionized water at 80 ℃ after being taken out, the mixture is continuously stirred for 8min, NdPO4 is deposited on the surface of the fiber fabric, and the surface of the fiber fabric with the coating is washed by the deionized water for 15s after being taken out, so that ions in the solution and loose solids on the surface are removed. And then, drying the fiber in an oven at 100 ℃ for 20min, then placing the fiber in a muffle furnace, carrying out heat treatment at 900 ℃ for 8min, then directly taking out the fiber, and carrying out immersion-heat treatment circulation for 5 times in such a way, thus finally preparing an NdPO4 interface phase on the surface of the fiber woven cloth. The final thickness of the interface phase is obtained by calculating the weight gain ratio and is 180-230 nm.
Example 3
Soaking the domestic zirconia fiber fabric in acetone for 1h, then placing the fabric in a muffle furnace for heat treatment at 600 ℃ for 1h, and removing the surface sizing agent for later use.
Cerium nitrate (Ce (NO3) 3.6H 2O), phosphoric acid and citric acid are magnetically stirred and mixed in deionization to prepare a precursor solution, wherein the concentration of the cerium nitrate is 55%. Then, the zirconia fiber fabric is immersed in the precursor solution for 15s and then taken out, the zirconia fiber fabric is taken out and then put into deionized water at 60 ℃, the mixture is continuously stirred for 15min, CePO4 is deposited on the surface of the fiber cloth, and the surface of the fiber cloth with the coating is washed by the deionized water for 10s after the zirconia fiber fabric is taken out, so that ions in the solution and loose solids on the surface are removed. And then, drying the fiber in an oven at 130 ℃ for 10min, then placing the fiber in a muffle furnace, carrying out heat treatment at 1000 ℃ for 5min, directly taking out the fiber, and carrying out immersion-heat treatment circulation for 7 times to finally prepare a CePO4 interface phase on the surface of the fiber woven cloth. The final thickness of the interface phase is obtained by weight gain calculation and is 260-290 nm.
Claims (6)
1. A preparation method of a continuous oxide fiber fabric surface coating is characterized by comprising the following steps:
the method comprises the following operation steps:
(1) pretreatment of continuous fiber preforms
Removing the sizing agent on the surface of the continuous fiber preform by a physical mode of high-temperature heat treatment or a chemical mode of solvent dissolution for later use;
(2) preparation of coating phase precursor solution
Preparing a coating precursor solution by a solution stirring and mixing mode, wherein the precursor solution is one or more of the following mixed solutions, namely a mixed solution of nitrate and phytic acid, a mixed solution of nitrate and phosphoric acid, a mixed solution of citric acid and a mixed solution of nitrate and ammonium dihydrogen phosphate, and the concentration of the nitrate in the coating precursor solution is 30-80%;
(3) continuous oxide fiber preform impregnation process
Immersing the pretreated continuous oxide fiber preform into the precursor solution for 10-20s, taking out, putting into deionized water at 50-100 ℃, continuously stirring for 5-15min, and washing the surface of the fiber cloth by the deionized water after taking out so as to remove ions in the solution and loose solids on the surface;
(4) drying and heat treatment process of coating
Drying the fiber preform impregnated with the precursor solution in an oven, and then placing the fiber preform in a muffle furnace for heat treatment, wherein the fiber preform impregnated with the precursor solution is dried in the oven at the drying temperature of 80-150 ℃ for 10-20min, the heat treatment temperature is 500-1100 ℃ and the heat treatment time is 3-10 min;
(5) control of coating thickness
And (4) repeatedly carrying out the steps (3) and (4) on the fiber preform after the heat treatment until a desired coating thickness is obtained.
2. The method for preparing the surface coating of the continuous oxide fiber fabric according to claim 1, wherein the adopted continuous oxide fiber comprises one or more of continuous alumina fiber, continuous mullite fiber, continuous zirconia fiber and continuous quartz fiber.
3. The method for preparing the surface coating of the continuous oxide fiber fabric according to claim 1, wherein the nitrate adopted in the preparation process of the precursor solution comprises one or more of lanthanum nitrate, neodymium nitrate and cerium nitrate.
4. The method as claimed in claim 1, wherein the nitrate concentration of the precursor solution is 50-60%.
5. The method for preparing the surface coating of the continuous oxide fiber fabric according to claim 1, wherein the time for immersing the continuous fiber preform into the precursor liquid is 15-20s, the continuous fiber preform is taken out and put into deionized water at 70-80 ℃, the mixture is continuously stirred for 10-15min, and the continuous fiber preform is taken out and put into the deionized water to wash the surface of the fiber preform for 15-20 s.
6. The method as claimed in claim 1, wherein the dried fiber preform is heat treated in a muffle furnace at 700-900 deg.C for 5-7 min.
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| CN109293367B (en) * | 2018-10-16 | 2021-08-31 | 航天特种材料及工艺技术研究所 | Cerium phosphate modified silicon carbide fiber reinforced silicon carbide composite material and preparation method thereof |
| CN110467439A (en) * | 2019-08-02 | 2019-11-19 | 中国航发北京航空材料研究院 | The preparation method of alumina fibre enhancing porous alumina ceramic based composites |
| CN111005226B (en) * | 2019-12-04 | 2022-07-05 | 航天特种材料及工艺技术研究所 | Method for modifying interface of three-dimensional fabric of alumina fiber and modified three-dimensional fabric of alumina fiber prepared by method |
| CN111039690B (en) * | 2019-12-26 | 2022-04-15 | 山东鲁阳浩特高技术纤维有限公司 | Alumina fiber composite module and preparation method thereof |
| CN113943168A (en) * | 2020-07-16 | 2022-01-18 | 南京航空航天大学 | Novel high-strength oxide ceramic matrix composite and preparation method thereof |
| CN113943169A (en) * | 2020-07-16 | 2022-01-18 | 南京航空航天大学 | SiC nanowire reinforced oxide ceramic matrix composite and preparation method thereof |
| CN113943164A (en) * | 2020-07-16 | 2022-01-18 | 南京航空航天大学 | Preparation method of novel high-strength oxide fiber preform |
| CN112125704A (en) * | 2020-09-23 | 2020-12-25 | 广东省科学院新材料研究所 | Silicon carbide fiber material with rare earth modified lanthanum phosphate coating and preparation method and application thereof |
| US20230406779A1 (en) * | 2020-09-23 | 2023-12-21 | Tosoh Corporation | Cover-layer-including ceramic continuous fiber, method for producing the same, ceramic matrix composite material and method for producing the same |
| CN114540991B (en) * | 2020-11-26 | 2023-09-29 | 山东工业陶瓷研究设计院有限公司 | Mullite fiber precursor oiling agent and preparation method thereof |
| CN113896538B (en) * | 2021-10-08 | 2023-03-17 | 江西信达航科新材料科技有限公司 | Preparation method of alumina fiber reinforced silicon carbide ceramic material and prepared alumina fiber reinforced silicon carbide ceramic material |
| CN114045671B (en) * | 2021-11-18 | 2024-01-09 | 航天特种材料及工艺技术研究所 | Continuous oxide fiber fabric with lanthanum phosphate layer and preparation method thereof |
| CN114044697B (en) * | 2021-11-18 | 2023-03-10 | 航天特种材料及工艺技术研究所 | Aluminum oxide fiber coated with lanthanum phosphate coating and preparation method and application thereof |
| CN115403397B (en) * | 2022-08-09 | 2023-10-24 | 西北工业大学 | Core-shell structure toughened (Hf, ta) C solid solution ultrahigh-temperature ceramic coating and one-step preparation method |
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| ES2688274T3 (en) * | 2005-06-30 | 2018-10-31 | Unifrax I Llc | Inorganic phosphate coated fiber and methods of preparation and use |
| CN102659442B (en) * | 2012-05-03 | 2014-07-02 | 南京航空航天大学 | Preparation method for oxide fiber toughened silicon dioxide ceramic-based composite material gap interface |
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Address after: 101300 Zhonghang Fucai No.1 scientific research building, aviation industrial park, Shunyi District, Beijing Patentee after: AVIC COMPOSITE Corp.,Ltd. Patentee after: AVIC BEIJING AERONAUTICAL MANUFACTURING TECHNOLOGY Research Institute Address before: 100024 Beijing city Chaoyang District eight Bridge North East Junzhuang No. 1 Patentee before: AVIC BEIJING AERONAUTICAL MANUFACTURING TECHNOLOGY Research Institute Patentee before: AVIC COMPOSITE Corp.,Ltd. |
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