WO2024098944A1 - Procédé de préparation de moule pour préforme composite à matrice céramique - Google Patents

Procédé de préparation de moule pour préforme composite à matrice céramique Download PDF

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Publication number
WO2024098944A1
WO2024098944A1 PCT/CN2023/118132 CN2023118132W WO2024098944A1 WO 2024098944 A1 WO2024098944 A1 WO 2024098944A1 CN 2023118132 W CN2023118132 W CN 2023118132W WO 2024098944 A1 WO2024098944 A1 WO 2024098944A1
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WIPO (PCT)
Prior art keywords
mold
parts
matrix composite
ceramic matrix
composite material
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PCT/CN2023/118132
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English (en)
Chinese (zh)
Inventor
涂建勇
陈静
刘梦珠
都嘉鑫
吴京军
李鹏
薛飞彪
吴亚明
Original Assignee
西安鑫垚陶瓷复合材料股份有限公司
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Publication of WO2024098944A1 publication Critical patent/WO2024098944A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B23/00—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/38—Treating surfaces of moulds, cores, or mandrels to prevent sticking

Definitions

  • the invention relates to a method for preparing a mold for a composite material preform, and in particular to a method for preparing a mold for a ceramic-based composite material preform.
  • Ceramic matrix composites are increasingly widely used in the aerospace field due to their excellent properties such as high strength, high stiffness, good fatigue resistance and designability of material layering.
  • the preparation processes of CMC-SiC ceramic composites mainly include slurry infiltration-hot pressing sintering, direct oxidation deposition (Direct Oxidation), chemical vapor infiltration (CVI), precursor polymer decomposition (Polymer Impregnation Pyrolysis, PIP), reactive melt infiltration (RMI), directional solidification (Directional Solidification), etc.
  • Different preparation methods have one thing in common, that is, molds are required to protect and fix the preforms during the preparation process.
  • molds are indispensable equipment and play an important role in the preparation of various complex structures and components of different sizes.
  • the structure of the mold and its connection method have an important influence on its performance.
  • For the design of the mold used in the shaping process of ceramic matrix composite components it is necessary to formulate its unique mold design principles according to different types of components.
  • the following points need to be considered during the mold design process: processing accessibility of complex surfaces, uniformity of component mold attachment, protection of components during demolding, and density uniformity during the subsequent chemical vapor deposition process.
  • the existing molds mainly adopt a combined mold structure, split the mold design, and use graphite bolts and nuts to connect the split molds.
  • This connection method is too complicated.
  • the mold needs to be connected with connectors, which increases the size, resulting in an increase in the mold processing cycle and time cost.
  • the wall thickness of the mold connector is thick, which affects the uniformity of the subsequent hot forming preparation process during the component preparation process, thereby affecting the final mechanical properties of the component.
  • Some structural molds are difficult to demold, not easy to operate, and will cause connection failure, resulting in deformation or even scrapping of the component during the subsequent preparation process, and are prone to mold damage, thereby increasing the cost of mold manufacturing and the component preparation cycle.
  • the purpose of the present invention is to solve the technical problems that the mold size of the existing ceramic matrix composite material preform is too large, the connection method is complicated, and the demoulding is difficult, which leads to deformation or even scrapping of the ceramic matrix composite material components.
  • a mold preparation method for a ceramic matrix composite material preform is proposed.
  • a method for preparing a mold for a ceramic matrix composite material preform which is special in that it comprises the following steps:
  • the outer mold includes at least two sub-outer molds; the sub-outer molds have an outer mold assembly surface for assembly, the outer mold assembly surfaces of two adjacent sub-outer molds are connected, and at least two sub-outer molds are assembled into an outer mold adapted to the ceramic-based composite material preform; and the outer mold assembly surface is provided with an outer mold positioning hole;
  • step S2 according to the mold designed in step S1, process the inner mold, each sub-outer mold and fasteners, the inner mold, sub-outer mold and fasteners are all made of graphite;
  • Each sub-outer mold is sleeved on the outside of the ceramic matrix composite material preform and fixed with fasteners for trial mold fitting, so that there is a reserved gap of 1-3 mm between the adjacent outer mold assembly surfaces, and the gap between the outer mold and the ceramic matrix composite material preform is measured at the same time. If the gap is less than 0.15 mm, the trial mold fitting is qualified; if the gap is ⁇ 0.15 mm, continue to lay carbon fiber cloth on the outside of the ceramic matrix composite material preform until the trial mold fitting is qualified;
  • step S8 repeat step S7, and pre-assemble the sub-outer mold.
  • pre-assembly use a three-dimensional coordinate measuring machine to measure the overall size of the mold until the profile tolerance is ⁇ 0.05mm.
  • the outer mold is assembled, and the fasteners are set on the outside of the outer mold to complete the mold closing;
  • step S9 after the mold is closed in step S8, it is fixed with fasteners, and then left to stand at room temperature and pressure for at least 24 hours, or dried at 200° C.-600° C. for 3-20 hours, to obtain a mold for a ceramic-based composite material preform.
  • step S7 the highest temperature of the effective working temperature range of the high-temperature adhesive is greater than the temperature at which the corresponding ceramic matrix composite material preform is deposited and prepared.
  • the inner mold includes at least two sub-inner molds, the sub-inner molds have inner mold assembly surfaces for assembly, and the inner mold assembly surfaces are provided with inner mold positioning holes;
  • step S2 processing the inner mold body is processing each sub-inner mold
  • step S3 the ceramic matrix composite material preform is shaped by laying carbon fiber cloth on the inner mold, specifically:
  • S3.2 Use high temperature adhesive to evenly coat the inner mold assembly surface. After coating the inner mold assembly surface with high temperature adhesive once, use a hot air gun adjusted to 100-150°C to blow the coated surface for no less than 50s;
  • step S3.3 Repeat step S3.2 and pre-assemble the sub-inner mold. After pre-assembly, use a three-dimensional coordinate measuring machine to detect the overall size of the mold until the outer contour tolerance is ⁇ 0.05mm, and the inner mold is assembled;
  • Carbon fiber cloth is laid on the inner mold assembled in step S3.3 to shape the ceramic matrix composite material preform, and the thickness of the laid carbon fiber cloth is 1.02-1.1 times the designed thickness of the ceramic matrix composite material preform.
  • step S3.2 the selection of the high-temperature adhesive: if the inner mold is first demoulded and then the outer mold is demoulded in the subsequent deposition preparation process of the ceramic matrix composite material preform corresponding to the mold, the effective working temperature of the high-temperature adhesive used for the outer mold assembly is higher than the effective working temperature of the high-temperature adhesive used for the inner mold assembly;
  • the effective working temperature of the high-temperature adhesive used in the outer mold assembly is lower than the effective working temperature of the high-temperature adhesive used in the inner mold assembly.
  • the high temperature adhesive used includes a first high temperature adhesive having an effective working temperature range of room temperature to 1200°C, a second high temperature adhesive having an effective working temperature range of room temperature to 1400°C, a third high temperature adhesive having an effective working temperature range of room temperature to 1600°C, or a fourth high temperature adhesive having an effective working temperature range of room temperature to 1800°C.
  • the first high temperature adhesive includes, by weight: 2-8 parts of PVA polyvinyl alcohol, 1-3 parts of borax, 2-6 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of N-N-methylenebisacrylamide, 5-10 parts of graphite powder, 70-78 parts of SiC powder, and 10-20 parts of water;
  • the second high temperature adhesive comprises, by weight: 4-15 parts of PVA polyvinyl alcohol, 1-5 parts of borax, 2-10 parts of aluminum dihydrogen phosphate, 2-5 parts of acrylamide, 2-5 parts of N-N-methylenebisacrylamide, 5-10 parts of graphite powder, 70-85 parts of SiC powder, and 10-20 parts of water;
  • the third high temperature adhesive comprises, by weight: 2-8 parts of PVA polyvinyl alcohol, 1-5 parts of borax, 2-10 parts of aluminum dihydrogen phosphate, 2-5 parts of acrylamide, 2-5 parts of N-N-methylenebisacrylamide, 1-2 parts of zirconium carbide, 5-10 parts of graphite powder, 70-85 parts of SiC powder, and 10-20 parts of water;
  • the fourth high-temperature adhesive includes, by weight: 4-15 parts of PVA polyvinyl alcohol, 1-5 parts of borax, 2-15 parts of aluminum dihydrogen phosphate, 2-5 parts of acrylamide, 2-5 parts of N-N-methylenebisacrylamide, 2-6 parts of zirconium carbide, 5-10 parts of graphite powder, 70-85 parts of SiC powder, and 10-20 parts of water.
  • the graphite is high-strength fine graphite, high-purity graphite or electrode graphite.
  • the ceramic matrix composite material preform is in the shape of a body of revolution, a box, a curved surface part, a blade part, a U-shaped part, an L-shaped part, a Z-shaped part, a W-shaped part, a special-shaped part or a flat plate part.
  • step S6 the outer mold assembly surface is cleaned and kept dry by using a handheld air gun to blow clean the assembly surface, then wiping it with a dust-free cloth soaked in ethanol, and leaving it to stand at room temperature and temperature for 5-10 minutes to allow it to dry fully.
  • the mold preparation method provided by the present invention adopts a high-temperature adhesive connection method, which can effectively reduce the area required for the bolt and nut connection method, reduce the weight of the overall mold device while improving the connection quality, and reduce the space occupied during the preparation of composite material components, thereby improving the preparation efficiency.
  • the present invention can select a suitable high-temperature adhesive according to the preparation process of the mold, so that the mold can be safely and conveniently removed without damaging the components and the mold, effectively improving the qualified rate of the components and the reuse rate of the mold, and reducing time and economic costs.
  • the preparation process of the present invention is simple and easy to operate.
  • the mold is a split structure, the mold size is reduced, the mold processing cycle is shortened, the economic cost is reduced, and the transportation efficiency and safety are improved.
  • the present invention selects different high-temperature adhesives to connect the molds through different process routes. Under the premise of avoiding deformation of components by preventing the failure of the high-temperature adhesive, the inner mold and the outer mold can be separated in a specific temperature working range, thereby improving the uniformity of component deposition and thus improving the final mechanical properties of the material.
  • the high-temperature adhesive connection method adopted in the present invention can effectively reduce the area required for the bolt and nut connection method, ensure the uniformity of the overall wall thickness of the mold, improve the deposition uniformity, and ensure the reliability of the prepared components.
  • the present invention adopts a high-temperature adhesive to connect the mold during the preparation of the composite material, thereby avoiding the deformation and scrapping of the component and the damage of the mold due to the failure of the mold connector, and ensuring the stability of the size and shape during the preparation of the component.
  • FIG1 is a schematic diagram of an embodiment of a box-type component preform in a mold preparation method for a ceramic-based composite material preform of the present invention
  • FIG2 is a schematic diagram of a mold design structure according to an embodiment of the present invention (fasteners are not shown);
  • FIG3 is a schematic diagram of the inner mold structure in an embodiment of the present invention.
  • FIG4 is a schematic diagram of an outer mold structure in an embodiment of the present invention.
  • FIG5 is a schematic diagram of the assembly surface structure 1 in an embodiment of the present invention.
  • FIG6 is a second schematic diagram of the assembly surface structure according to an embodiment of the present invention.
  • FIG. 7 is a schematic diagram of the assembly structure of the mold and the preform in an embodiment of the present invention.
  • 1-ceramic matrix composite material preform 2-inner mold, 3-sub-outer mold, 4-outer mold assembly surface, 5-detection reference hole, 6-limiting groove, 9-outer mold positioning hole, 10-fastener.
  • This embodiment provides a method for preparing a mold for a ceramic matrix composite material preform. Taking a box-type preform as an example, the method includes the following steps:
  • the mold includes an inner mold 2, an outer mold and a fastener 10.
  • the inner mold 2 and the outer mold are designed to have the same thickness.
  • the inner mold 2 is an integrated structure, and the outer mold includes two sub-outer molds 3.
  • the sub-outer molds 3 have an outer mold assembly surface 4 for assembly to form an outer mold that matches the ceramic-based composite material preform 1.
  • An outer mold positioning hole 9 is provided on the outer mold assembly surface 4.
  • step S2 According to the mold designed in step S1, the inner mold 2, each sub-outer mold 3 and the fastener 10 are processed.
  • the materials of the inner mold 2, the sub-outer mold 3 and the fastener 10 are all graphite, and the graphite adopts high-strength fine graphite, high-purity graphite or electrode graphite.
  • the inner mold 2 and the sub-outer mold 3 are provided with detection reference holes 5 for detecting the processed inner mold 2 and the sub-outer mold 3 to confirm whether they meet the use requirements.
  • each sub-outer mold 3 is sleeved on the outside of the ceramic-based composite material preform 1 and fixed with fasteners 10 for trial mold fitting, so that there is a reserved gap of 1-3 mm between adjacent outer mold assembly surfaces 4, and a 0.15 mm feeler gauge is used to measure the gap between the outer mold and the ceramic-based composite material preform 1. If the gap is less than 0.15 mm, the trial mold fitting is qualified; if the gap is ⁇ 0.15 mm, continue to lay carbon fiber cloth on the ceramic-based composite material preform 1 until the trial mold fitting is qualified.
  • the effective working temperature range of the high-temperature adhesive is room temperature-1800°C.
  • the high-temperature adhesive includes a first high-temperature adhesive with an effective working temperature range of room temperature-1200°C, a second high-temperature adhesive with an effective working temperature range of room temperature-1400°C, a third high-temperature adhesive with an effective working temperature range of room temperature-1600°C, and a fourth high-temperature adhesive with an effective working temperature range of room temperature-1800°C.
  • the first high-temperature adhesive includes, by weight: 2-8 parts of PVA polyvinyl alcohol, 1-3 parts of borax, 2-6 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of NN-methylenebisacrylamide, 5-10 parts of graphite powder, 70-78 parts of SiC powder, and 10-20 parts of water.
  • the second high-temperature adhesive includes, by weight: 4-15 parts of PVA polyvinyl alcohol.
  • the third high-temperature adhesive includes: 2-8 parts of PVA polyvinyl alcohol, 1-5 parts of borax, 2-10 parts of aluminum dihydrogen phosphate, 2-5 parts of acrylamide, 2-5 parts of NN-methylenebisacrylamide, 1-2 parts of zirconium carbide, 5-10 parts of graphite powder, 70-85 parts of SiC powder, and 10-20 parts of water;
  • the fourth high-temperature adhesive calculated by weight, includes: 4-15 parts of PVA polyvinyl alcohol, 1-5 parts of borax, 2-15 parts of aluminum dihydrogen phosphate, 2-5 parts of acrylamide, 2-5 parts of NN-methylenebisacrylamide, 2-6 parts of zirconium carbide, 5-10 parts of graphite powder, 70-85
  • High-temperature adhesives will debond at temperatures higher than the effective working temperature range, because graphite powder begins to oxidize at 600°C in an air atmosphere, and the oxidation reaches a peak at about 800°C. When the oxidation phenomenon continues, the adhesive strength of the adhesive decreases, thereby achieving debonding.
  • the highest temperature of the effective working temperature range of the high-temperature adhesive is selected to be greater than the temperature at which the corresponding ceramic-based composite material preform 1 is deposited and prepared; after the high-temperature adhesive on the outer mold assembly surface 4 is coated once, a hot air gun is used to adjust the temperature to 100-150°C to blow the surface for no less than 50 seconds until there is no stickiness on the connection surface; during the brushing process, the principle of from top to bottom, from left to right, inside first and then outside, difficult first and then easy, and criss-crossing should be followed, and there should be no sagging phenomenon and no visible solution accumulation.
  • step S8 Repeat step S7 and pre-assemble the sub-outer mold 3 to ensure that the upper and lower molding surfaces and the end surface interfaces between the molds are flush, and the limit groove 6 on the inner mold 2 is flush with the upper surface of the preform without obvious steps or gaps; after pre-assembly, use a three-coordinate measuring instrument to measure the overall size of the mold until the outer contour tolerance is ⁇ 0.05mm. The outer mold is assembled, and then the fastener 10 is set on the outside of the outer mold 3 to complete the mold closing.
  • step S9 after the mold is fixed by fasteners 10 after the mold is closed in step S8, it is left to stand at least 24 hours at room temperature and pressure, or dried at 200°C-600°C for 3-20 hours, and the high-temperature adhesive is cured to obtain a mold for the ceramic-based composite material preform 1; the subsequent processing can be carried out.
  • the two high-temperature adhesive curing methods can be flexibly selected according to time requirements.
  • the inner mold 2 may include a plurality of sub-inner molds, each of which has an inner mold assembly surface for assembly, and an inner mold positioning hole is provided on the inner mold assembly surface; in step S2, processing the inner mold 2 specifically includes processing each sub-inner mold; in step S3, the ceramic matrix composite material preform 1 is shaped by laying a carbon fiber cloth on the inner mold 2, specifically:
  • S3.2 Use high-temperature adhesive to evenly coat the inner mold assembly surface. After the high-temperature adhesive on the inner mold assembly surface is coated once, use a hot air gun adjusted to 100-150°C to blow and brush the coated surface for not less than 50s; the selection of high-temperature adhesive here needs to consider the working environment temperature of the subsequent processing of the preform.
  • the effective working temperature of the high-temperature adhesive used for outer mold assembly is higher than the effective working temperature of the high-temperature adhesive used for inner mold assembly; if the subsequent deposition preparation process of the ceramic-based composite material preform 1 corresponding to the mold first performs outer mold demolding and then inner mold 2 demolding, the effective working temperature of the high-temperature adhesive used for outer mold assembly is lower than the effective working temperature of the high-temperature adhesive used for inner mold assembly.
  • step S3.3 Repeat step S3.2 and pre-assemble the sub-inner mold 2. After pre-assembly, use a three-dimensional coordinate measuring machine to detect the overall size of the mold until the outer contour tolerance is ⁇ 0.05mm, and the inner mold 2 is assembled;
  • the first step of the shaping operation is to calculate and cut the fiber cloth.
  • the amount of fiber cloth required for the maximum outer size of the box-shaped part is calculated, and an appropriate lock edge margin is reserved. The reserved amount is not less than 10 mm from the end face of the preform to the inner and outer molds.
  • the fiber cloth is cut according to the calculated size.
  • the cut fiber cloth is flanged layer by layer on the mold surface used by the inner mold component, and the components are laid and flanged layer by layer.
  • There are two main flanging methods for the box-shaped part namely right-angle flanging and bevel flanging.
  • the thickness of the laid carbon fiber cloth is 1.02-1.1 times the design thickness of the ceramic-based composite material preform 1.
  • the above embodiment is based on a box-type ceramic-based composite preform 1.
  • the mold preparation method provided by the present invention is also applicable to rotating bodies, box bodies, curved parts, blade parts, U-shaped parts, L-shaped parts, Z-shaped, W-shaped, special-shaped parts or flat parts, etc.; the mold preparation method can avoid the need for additional connection structure design for existing mechanical connections (for example, structures such as flanges and connection flanges that need to be designed for connection), reduce the weight and volume of the mold, and at the same time, when demolding, it only needs to heat the mold and the ceramic-based composite preform 1 as a whole to above the effective working temperature of the high-temperature adhesive used, and the mold can be automatically demolded, thereby avoiding damage to the mold and the preform when demolding by mechanical connection, reducing costs, facilitating operation, and effectively changing the uniformity of the component in the subsequent deposition preparation process, thereby improving the mechanical properties of the component.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)

Abstract

La présente invention concerne un procédé de préparation de moule pour une préforme composite à matrice céramique, destiné à résoudre les problèmes techniques de déformation et même de mise au rebut d'un composant composite à matrice céramique provoqués par une dimension excessive de moule, un mode de raccordement complexe et un démoulage difficile d'une préforme composite à matrice céramique existante. Le procédé comprend les étapes consistant à : 1, concevoir un moule ; 2, usiner le moule ; 3, effectuer une mise en forme de préforme composite à matrice céramique sur un moule interne ; 4, effectuer une fermeture de moule d'essai de moules sous-externes, la fermeture de moule d'essai étant réussie si un interstice réservé de 1 à 3 mm est formé entre des surfaces d'ensemble de moule externes adjacentes et un interstice entre un moule externe et la préforme composite à matrice céramique est inférieur à 0,15 mm ; 5, piquer la préforme composite à matrice céramique et le moule interne ; 6, prétraiter les surfaces d'ensemble de moule externe ; 7, brosser sur un adhésif à haute température et préassembler jusqu'à ce que la tolérance de profil soit de ± 0,05 mm ; et 8, durcir l'adhésif à haute température pour obtenir un moule pour la préforme composite à matrice céramique.
PCT/CN2023/118132 2022-11-11 2023-09-12 Procédé de préparation de moule pour préforme composite à matrice céramique WO2024098944A1 (fr)

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CN202211420886.6 2022-11-11
CN202211420886.6A CN115674424A (zh) 2022-11-11 2022-11-11 一种用于陶瓷基复合材料预制体的模具制备方法

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CN115674424A (zh) * 2022-11-11 2023-02-03 西安鑫垚陶瓷复合材料股份有限公司 一种用于陶瓷基复合材料预制体的模具制备方法

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CN115674424A (zh) * 2022-11-11 2023-02-03 西安鑫垚陶瓷复合材料股份有限公司 一种用于陶瓷基复合材料预制体的模具制备方法

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