JP2019195938A - Method for producing prepreg sheet for pressurization-hot molding of 2d-ceramic fiber-reinforced composite material with cylinder shape - Google Patents

Method for producing prepreg sheet for pressurization-hot molding of 2d-ceramic fiber-reinforced composite material with cylinder shape Download PDF

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JP2019195938A
JP2019195938A JP2018090952A JP2018090952A JP2019195938A JP 2019195938 A JP2019195938 A JP 2019195938A JP 2018090952 A JP2018090952 A JP 2018090952A JP 2018090952 A JP2018090952 A JP 2018090952A JP 2019195938 A JP2019195938 A JP 2019195938A
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prepreg sheet
composite material
pressurization
cylinder
molding
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晃 香山
Akira Kayama
晃 香山
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Nite Co Ltd
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Nite Co Ltd
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Abstract

To suppress characteristic deterioration caused by thread breakage in reinforcing ceramic fiber as a component of prepreg sheets as an intermediate stock for producing a ceramic composite material upon molding by heating-pressurization by molding a preform according to the lamination of the prepreg sheets.SOLUTION: A prepreg sheet as an intermediate stock for producing a ceramic composite material is subjected to corrugation working (corrugation shape application), and the same is laminated to mold a preform, thus the thread breakage of reinforcing ceramic fiber caused by volume shrinkage in heating-pressurization is suppressed.SELECTED DRAWING: Figure 1

Description

本発明は、シリンダー形状の2D-セラミック繊維強化複合材料の加圧・加熱成形用プリプレグシートの製造方法に関するものである。   The present invention relates to a method for producing a prepreg sheet for pressurizing and thermoforming a cylindrical 2D-ceramic fiber reinforced composite material.

シリンダー形状の2方向(2D)セラミック繊維強化複合材料製造において高密度、高結晶性を達成できる製造法としてNITE法(関連特許に示す)がある。この方法で作成するには中間素材としてプリプレグシートを用いて、プリフォームを作成し、プリフォームの加圧・加熱により成形し、最終製品を作成する。従来技術であるNITE法プリプレグシートでシリンダー形状の2D-セラミック繊維強化複合材料製品を作成する場合、加圧・加熱成形時の体積収縮により肉厚が減少し、内側表面に向かって周長が大きく増加する。この際、セラミック繊維はこの製造条件では塑性変形を行わないので部分的に断線することになり、強度低下の原因となり、シリンダーの大型化における大きな問題であった。   The NITE method (shown in related patents) is a production method that can achieve high density and high crystallinity in the production of a cylinder-shaped bi-directional (2D) ceramic fiber reinforced composite material. In order to produce by this method, a preform is produced using a prepreg sheet as an intermediate material, and is molded by pressurizing and heating the preform to produce a final product. When creating a cylindrical 2D-ceramic fiber reinforced composite material product using the conventional NITE prepreg sheet, the wall thickness decreases due to volume shrinkage during pressure and heat molding, and the perimeter increases toward the inner surface. To increase. At this time, since the ceramic fiber does not undergo plastic deformation under the manufacturing conditions, it is partially broken, which causes a decrease in strength and is a big problem in increasing the size of the cylinder.

大型のシリンダーを作成する場合には加圧・加熱成型時における体積収縮に伴うプリプレグシートの肉厚減少と長さの増加が起こる。前者はマトリックス成分の高密度化によるものであり、ナノ粉末を主成分とするマトリックスは十分な変形能力を有し、高密度・高結晶性のマトリックス形成は実現する。一方、長さの増加にはマトリックス部分の変形には問題は無いが、セラミック繊維はこの成型条件では変形せず、繊維が破断してマトリックス変形に対応する事になり、大型化に伴いこの弊害は大きくなる傾向にある。図1は、従来法でのプリプレグシートを用いたプリフォームでの成型時に起こる現象を示している。1は一方向プリプレグシートであり、交互に繊維方向を変えて積層する状況を2に示す。積層プロイプレグシートは芯材に巻かれプリフォームとなり、芯材を取り外したプリフォームを製品外径に合わせたダイスに挿入した状態が3である。3の状態で、内圧をかけて、加熱することにより成型する。この際、繊維が十分な延性を有しないために断線する様子が4に示されている。これが特性劣化を引き起こすという、この方式の欠点であった。   When making a large cylinder, the thickness and length of the prepreg sheet decrease due to volume shrinkage during pressurization and heat molding. The former is due to the densification of the matrix components, and the matrix mainly composed of nanopowder has a sufficient deformation capacity, and a high-density and highly crystalline matrix can be formed. On the other hand, there is no problem in the deformation of the matrix part due to the increase in length, but the ceramic fiber does not deform under this molding condition, and the fiber breaks to cope with the matrix deformation. Tend to grow. FIG. 1 shows a phenomenon that occurs during molding of a preform using a prepreg sheet in a conventional method. Reference numeral 1 denotes a unidirectional prepreg sheet, and FIG. The laminated ploypreg sheet is wound around a core material to form a preform, and the state in which the preform with the core material removed is inserted into a die matched to the outer diameter of the product is 3. In the state of 3, it is molded by applying internal pressure and heating. In this case, 4 shows a state in which the fiber is disconnected because it does not have sufficient ductility. This is a drawback of this method that causes deterioration of characteristics.

大型のシリンダー作製におけるこの欠点はシリンダーに求められる強度特性確保の上で大きな障害となる。具体的には、この欠点を補うためにより多くの繊維強化を施す必要がおこり、価格面、重量面での本材料の優位性を大きく損なうものであった。   This drawback in the production of large cylinders is a major obstacle to ensuring the strength characteristics required for the cylinder. Specifically, it is necessary to reinforce more fibers to compensate for this drawback, which greatly impairs the superiority of the material in terms of price and weight.

この改善策として、プリプレグシートにコルゲート加工(波打形状付与)を施す方法を考案した。このプリプレグシート(以下、波打プリプレグシート)を用いることにより、大型シリンダーの製造時においても波形の繊維が成型時に伸直性示す事で、必要とされる周長の増加に対応出来、真円状の製品断面内において同心円を描く繊維強化構造を達成できる。図2はこの方法による大型シリンダーの成形過程を示すための説明図であり、シリンダーの断面方向での説明図である。図2で、5は波打プリプレグシート、6は波打プリプレグシートを貼り付けた管状プリフォームである。この管状プリフォームを内圧により成型することにより糸切れのない、大型シリンダーの製造が可能になる事を7に示す。しかしながらこの方法でも、プリフォーム形状や成型時での収縮率等を的確に設計し、必要最低限の波打形状を付与させることが必要であり、このための繊維特性、マトリックス成分となる成分の設計は重要である。   As an improvement measure, we devised a method for corrugating the prepreg sheet. By using this prepreg sheet (hereinafter referred to as undulating prepreg sheet), even when manufacturing large cylinders, the corrugated fibers show straightness during molding, so that the required circumference can be increased. The fiber reinforced structure which draws a concentric circle in the cross section of the product can be achieved. FIG. 2 is an explanatory diagram for illustrating a molding process of a large cylinder by this method, and is an explanatory diagram in a cross-sectional direction of the cylinder. In FIG. 2, 5 is a corrugated prepreg sheet, and 6 is a tubular preform with a corrugated prepreg sheet attached thereto. It is shown in 7 that it is possible to produce a large cylinder without thread breakage by molding this tubular preform with internal pressure. However, even with this method, it is necessary to accurately design the preform shape and the shrinkage rate at the time of molding, and to give the minimum necessary corrugated shape. For this purpose, the fiber characteristics, the component of the matrix component Design is important.

特許第4536950号Patent No. 4536950

従来技術であるNITE法プリプレグシートでシリンダー形状のシリンダー形状の2D-セラミック繊維強化複合材料製品を作成する場合の問題点である、加圧・加熱成形時の体積収縮により肉厚が減少し、内側表面に向かって周長が大きく増加する結果、セラミック繊維は断線することになり、強度低下の原因となる。この発明は、コルゲート加工(波状形状付与)されたプリプレグシートを作成することにより必要とされる周長の増加に対応出来、真円状の製品断面内において同心円を描く繊維強化構造を達成できる。   Thickness decreases due to volumetric shrinkage during pressure and heat forming, which is a problem when creating a cylinder-shaped 2D-ceramic fiber reinforced composite material product using the conventional NITE prepreg sheet. As a result of the large increase in the circumference toward the surface, the ceramic fibers are disconnected, causing a decrease in strength. The present invention can cope with an increase in circumference required by producing a prepreg sheet that has been corrugated (provided with a corrugated shape), and can achieve a fiber-reinforced structure that draws concentric circles within a perfectly circular product cross section.

解決しようとする問題点は、大型シリンダーの成型時において繊維が破断し、十分な強度が得られない点である。   The problem to be solved is that the fiber breaks when a large cylinder is molded, and sufficient strength cannot be obtained.

本発明は、NITE法によるセラミック複合材料の大型シリンダーまたは類似の形状の製品の中間素材であるプリプレグシートにコルゲート加工(波打形状付与)を施す方法とこの中間素材を用いて大型のセラミック複合材料シリンダーを製造する事を特徴とする。   The present invention relates to a method for corrugating (providing a corrugated shape) to a prepreg sheet, which is an intermediate material of a ceramic composite material large cylinder or a similar shaped product by the NITE method, and a large ceramic composite material using the intermediate material It is characterized by manufacturing a cylinder.

本発明のコルゲート加工(波打形状付与)されたプリプレグシートを用いることにより大型シリンダーや類似の形状の製品を2方向強化セラミック複合材料で製造する際の繊維破断という問題を解決できるという利点がある。   By using the prepreg sheet that has been corrugated (provided with corrugated shape) according to the present invention, there is an advantage that the problem of fiber breakage when a large-sized cylinder or a product having a similar shape is produced with a bi-directional reinforced ceramic composite material can be solved .

図1は従来法のNITE法プリプレグシートを用いる2D-繊維強化セラミック複合材料製シリンダーの成形過程を示す説明図である。(実施例1)FIG. 1 is an explanatory view showing a molding process of a 2D-fiber reinforced ceramic composite cylinder using a conventional NITE prepreg sheet. Example 1 図2は本発明品であるコルゲート加工(波打形状付与)されたプリプレグシートを用いることにより大型シリンダーや類似の形状の製品を2方向強化セラミック複合材料で製造する過程を示す説明図である。(実施例2)FIG. 2 is an explanatory view showing a process of manufacturing a large cylinder or a product having a similar shape with a bi-directionally reinforced ceramic composite material by using a prepreg sheet that has been corrugated (giving a corrugated shape) according to the present invention. (Example 2) 図3は従来法のNITE法プリプレグシートを用いる2D-繊維強化セラミック複合材料製シリンダーの成形例であり、糸切れが明確に認められる。本発明法でのプリプレグシートを用いた製品では糸切れは認められず、平滑なシリンダー表面が得られている。FIG. 3 is a molding example of a cylinder made of 2D-fiber reinforced ceramic composite material using a conventional NITE prepreg sheet, and yarn breakage is clearly recognized. In the product using the prepreg sheet in the method of the present invention, yarn breakage is not recognized, and a smooth cylinder surface is obtained. 図4は本発明品であるコルゲート加工(波打形状付与)されたプリプレグシートを用いるシリンダーの成形例であり、断面拡大図(左下)では伸直した繊維配列が認められる。また、糸切れは認められない。FIG. 4 is an example of forming a cylinder using a prepreg sheet that has been corrugated (giving a corrugated shape), which is a product of the present invention. In the enlarged cross-sectional view (lower left), a straightened fiber array is observed. Moreover, thread breakage is not recognized.

従来の製品である直径10mmの環状製品に比して径が大きい直径40mmのシリンダーを内圧式により成型を実現させた。   A cylinder having a diameter of 40 mm, which is larger than the conventional annular product having a diameter of 10 mm, was molded by an internal pressure method.

図1は、本発明の前提となるNITE法による従来法のプリプレグシートでのシリンダー製造の過程を示す、実施例の断面図(概念)であって、1〜2は、図2と同様である。   FIG. 1 is a cross-sectional view (concept) of an embodiment showing a process of manufacturing a cylinder using a conventional prepreg sheet by the NITE method as a premise of the present invention. .

図2は本発明での大型シリンダー製造過程の概念を説明している。波打プリプレグシート5はプリフォーム状態での径方向の長さに対応する波打プリプレグ中の実際の繊維長さと成型後の径方向の繊維長さが一致するように設計される。プリフォーム6はこのように設計された波打プリプレグシートを管状プリフォームに成型し、内圧式で成型する際のブロックに挿入した状態を示す。内圧式による成型で大型シリンダーを成型した状態が7であり、プリフォームの際の肉厚が大きく減少していること、波打っている繊維がまっすぐに伸びているが断線のない事を示している。   FIG. 2 illustrates the concept of the large cylinder manufacturing process in the present invention. The corrugated prepreg sheet 5 is designed so that the actual fiber length in the corrugated prepreg corresponding to the radial length in the preform state matches the radial fiber length after molding. The preform 6 shows a state in which a corrugated prepreg sheet designed in this way is molded into a tubular preform and inserted into a block when molded by an internal pressure type. 7 shows that the large cylinder is molded by internal pressure molding, the thickness of the preform is greatly reduced, and the wavy fibers are straight but not broken. Yes.

実施例としてSiC/SiC複合材料製のシリンダーの断面組織を図3に示す。また、製品の外観を図4に示す。   As an example, a cross-sectional structure of a cylinder made of SiC / SiC composite material is shown in FIG. Fig. 4 shows the appearance of the product.

優れた強度特性、特にセラミック材料としての高強度とセラミック材料の欠点である脆性を改善させ、擬延性を示す大型シリンダー材は超高温や高腐食性雰囲気その他の苛酷環境用の材料として強度部材のみならず、機能材料としての役割も併せ持つ材料として幅広い分野での用途が考えられる。特に、NITE法での特徴である高結晶性と高密度に由来する優れた気密性は他のセラミック複合材料では実現できない水準にあり、原子力・核融合分野、超臨界地熱発電に代表される再生エネルギー分野での優れた耐環境性などが不可欠な用途にも適用できる。   Large cylinder material that exhibits excellent strength characteristics, especially high strength as a ceramic material and brittleness, which is a drawback of ceramic materials, and exhibits pseudo-ductility is only a strength member as a material for ultra-high temperature, highly corrosive atmosphere and other harsh environments In addition, it can be used in a wide range of fields as a material that also has a role as a functional material. In particular, the excellent crystallinity and high airtightness derived from high density, which are the characteristics of the NITE method, are at a level that cannot be achieved with other ceramic composite materials. Regeneration represented by nuclear and nuclear fusion fields and supercritical geothermal power generation. It can also be used in applications where excellent environmental resistance in the energy field is essential.

1 一方向プリプレグシート
2 積層プリプレグシート
3 通常方式での管状プリフォーム
4 内圧による拡管(糸切れ)
5 波打プリプレグシート
6 波打プリプレグシート貼り付け管状プリフォーム
7 内圧による拡管(糸切れなし)
DESCRIPTION OF SYMBOLS 1 Unidirectional prepreg sheet 2 Laminated prepreg sheet 3 Tubular preform by a normal system 4 Pipe expansion by internal pressure (thread breakage)
5 Corrugated prepreg sheet 6 Tubular preform with corrugated prepreg sheet 7 Tube expansion by internal pressure (no thread breakage)

Claims (2)

繊維強化セラミック複合材料でシリンダーまたは類似の形状の製品を作成する際に加熱・加圧を用いる成型に用いられる中間素材であるプリプレグシートにコルゲート加工(波打形状付与)を施す方法   A method of corrugating (providing corrugated shape) to a prepreg sheet, which is an intermediate material used for molding using heating and pressurization when creating a cylinder or similar shaped product with a fiber reinforced ceramic composite material 請求項1のプリプレグシートを用いてプリフォームを作成し、これを用いて繊維強化セラミック複合材料でシリンダーまたは類似の形状の製品を作成する事。 A preform is prepared using the prepreg sheet according to claim 1, and a cylinder or a similar shaped product is formed using the fiber reinforced ceramic composite material.
JP2018090952A 2018-05-09 2018-05-09 Method for producing prepreg sheet for pressurization-hot molding of 2d-ceramic fiber-reinforced composite material with cylinder shape Pending JP2019195938A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113293475A (en) * 2020-12-25 2021-08-24 河南省西峡开元冶金材料有限公司 Ceramic fiber pretreatment method and manufacturing method of ceramic fiber gasket
CN114907127A (en) * 2022-05-09 2022-08-16 厦门大学 Matrix-modified SiC/SiC composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113293475A (en) * 2020-12-25 2021-08-24 河南省西峡开元冶金材料有限公司 Ceramic fiber pretreatment method and manufacturing method of ceramic fiber gasket
CN114907127A (en) * 2022-05-09 2022-08-16 厦门大学 Matrix-modified SiC/SiC composite material and preparation method thereof

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