CN114014678B - 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法 - Google Patents

一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法 Download PDF

Info

Publication number
CN114014678B
CN114014678B CN202111563860.2A CN202111563860A CN114014678B CN 114014678 B CN114014678 B CN 114014678B CN 202111563860 A CN202111563860 A CN 202111563860A CN 114014678 B CN114014678 B CN 114014678B
Authority
CN
China
Prior art keywords
carbon
flat plate
density
fiber
composite material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111563860.2A
Other languages
English (en)
Other versions
CN114014678A (zh
Inventor
陈腾飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Central South University
Original Assignee
Central South University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central South University filed Critical Central South University
Priority to CN202111563860.2A priority Critical patent/CN114014678B/zh
Publication of CN114014678A publication Critical patent/CN114014678A/zh
Application granted granted Critical
Publication of CN114014678B publication Critical patent/CN114014678B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/024—Woven fabric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/022—Non-woven fabric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B32B2260/023—Two or more layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Ceramic Products (AREA)
  • Laminated Bodies (AREA)

Abstract

本发明提供一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法，属于单晶硅炉和类单晶铸锭炉及炭基复合材料领域。该复合材料平板通过预制件经热压成型、碳化、石墨化制得。该预制件包括：中间层和与其交替叠加针刺的表面层；所述中间层由面密度为280～600g/m2的炭纤维平纹布或斜纹布加面密度为80～120g/m2的短纤维网胎交替叠层针刺而成；所述表面层由面密度180～300g/m2的石英纤维无纬布加面密度为60～120g/m2短石英纤维网胎交替叠加针刺而成。所得复合材料平板强度高，可以有效降低表面层与硅蒸气反应速度和反应程度，适用于高效单晶炉保温盖板和类单晶铸锭炉的盖板、顶板及坩埚护板等。

Description

一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法
技术领域
本发明涉及单晶硅炉和类单晶铸锭炉及炭基复合材料领域，具体涉及一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法。
背景技术
炭/炭复合材料是一种炭纤维增强炭基体复合材料，具有密度低、比强度高、耐高温、热膨胀系数小、尺寸稳定性好、结构可设计性强、耐腐蚀等优异性能而广泛应用于军工和民用领域，特别是随着技术进步、制造成本降低，在制造大规格产品和结构可设计性强等方面的优势，近些年炭/炭复合材料在大型单晶硅炉和类单晶铸锭炉的热场部件上的应用非常广泛，其中，炭/炭复合材料保温盖板和顶板、盖板是其中热场系统的关键部件之一。
在单晶硅拉制和铸锭类单晶时，热场部件处于硅蒸气和惰性气体的混合气氛中，硅会在热场表面沉积并部分与热场用炭/炭复合材料或石墨材料表面反应生成碳化硅或者渗透到表面一定深度的孔隙中与炭反应生成碳化硅，由于碳化硅与炭/炭或石墨的热膨胀系数不匹配，容易脱落和粉化，从而影响热场部件的进一步使用，进而影响热场部件的使用寿命。而且单晶炉的保温盖板和类单晶铸锭炉的盖板和顶板直面硅料，如果表面炭或碳化硅粉化脱落，会严重影响产品质量。因此，亟需解决单晶炉的保温盖板和类单晶铸锭炉的盖板和顶板的表面，降低硅蒸气对上述平板的表面影响。
发明内容
针对现有技术中单晶炉保温盖板和类单晶铸锭炉的盖板和顶板容易受硅蒸气硅化影响的弊端，本发明提供一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法，用于制备单晶炉保温盖板和类单晶铸锭炉的顶板和盖板，使得板材的表面与硅蒸气基本不反应，并降低表面的碳含量。
本发明提供了一种石英纤维/炭纤维增强炭基复合材料平板预制件，该预制件包括：中间层和与所述中间层上下表面通过交替叠加针刺连接的表面层；所述中间层由面密度为280～600g/m2的炭纤维平纹布或斜纹布加面密度为80～120g/m2的短纤维网胎交替叠层针刺而成；所述表面层由面密度180～300g/m2的石英纤维无纬布加面密度为60～120g/m2短石英纤维网胎交替叠加针刺而成。
优选地，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1～7∶3，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4～9∶1，密度0.4～0.6g/cm3。
本发明还提供了一种石英纤维/炭纤维增强炭基复合材料平板，该平板使用上述的预制件制得。
本发明还提供了一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，包括以下步骤：
S1、预制件的制备：按重量比将面密度为280～600g/m2的炭纤维平纹布或斜纹布加面密度为80～120g/m2的短纤维网胎交替叠层针刺而得到中间层；在中间层表面由面密度180～300g/m2的石英纤维无纬布加面密度为60～120g/m2短石英纤维网胎按重量比交叠层针刺成表面层；翻转后，在中间层另一表面由面密度180～300g/m2的石英纤维无纬布加面密度为60～120g/m2短石英纤维网胎按重量比交叠层针刺成另一表面层，得到预制件；
S2、预制件的热压成型：将步骤S1得到的预制件喷淋或浸渍树脂，置于不锈钢板上阴干，将不锈钢板和预制件推送至平板热压机热压成型，冷却至室温，得到密度为1.3～1.6g/cm3的第一平板坯；
S3、碳化：将步骤S2制得的第一平板坯放入碳化炉中碳化，每块平板坯间垫一层硫酸纸或牛皮纸，每1块～15块平板坯隔一块50～100mm厚的石墨或炭/炭复合材料标准平板，最上面再压一块石墨或炭/炭复合材料标准平板，避免碳化时变形，得到密度为1.0～1.3g/cm3的第二平板坯；将第二平板坯通过浸渍树脂或沥青，再碳化，得到密度为1.4～1.6g/cm3的第三平板坯；
S4、石墨化：将表面清理后的第三平板坯装入石墨化炉进行高温处理，每块平板坯间垫一层硫酸纸或牛皮纸，每1块～15块平板坯隔一块50～100mm厚的石墨或炭/炭复合材料标准平板，最上面再压一块石墨或炭/炭复合材料标准平板，避免石墨化时变形，得到石英纤维表面部分转化为碳化硅的石英纤维/炭纤维增强炭基复合材料平板。
根据使用需求加工至规定尺寸。用于高效单晶炉保温盖板和类单晶铸锭炉的盖板、顶板及坩埚护板等。
优选地，步骤S1中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1～7∶3，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4～9∶1，密度0.4～0.6g/cm3。
优选地，其特征在于，步骤S2中，所述树脂包括酚醛树脂或呋喃树脂中的任意一种。还可以是其他残炭率较高的树脂。
优选地，步骤S2中，所述热压成型具体为：将不锈钢平板和浸渍树脂的预制件推送到平板热压机，垫好限高块，温度控制在150～300℃，待温度升到树脂粘度增大，树脂基本不外流时，加压，压力为50～600t，与限高块等高时，保压，升温到设定温度200～220℃，保温，2～3小时，继续保压，自然冷却到室温。
优选地，步骤S3中，所述第二平板坯还可通过化学气相沉积增密工艺而得到第三平板坯。
优选地，步骤S4中，所述高温处理的温度为1300～1800℃，时间为3～15小时。
本发明中石英纤维与基体炭界面处，在高温下发生反应，反应方程式为：SiO2+2C＝Si+2CO；Si+C＝SiC；反应生成碳化硅界面层以后，进一步反应比较困难，因此，只有石英纤维表面部分转化成碳化硅；由于上下表面层以石英纤维+碳化硅+基体炭组成，降低了炭含量，同时降低了硅蒸气与平板表面的反应速度和反应程度，有利于提高平板的使用寿命。
本发明制备的石英纤维/炭纤维增强炭基复合材料平板可适用于高效单晶炉保温盖板和类单晶铸锭炉的盖板、顶板及坩埚护板等。
本发明技术方案，具有如下优点：
本发明设计制备的一种石英纤维/炭纤维增强炭基复合材料平板，预制件的的中间层为炭纤维，上下表面层为石英纤维组成，分别采用炭纤维平纹布或斜纹布加段炭纤维网胎交替叠层针刺或石英纤维无纬布+短石英纤维网胎交替叠层针刺而成石英纤维/炭纤维复合预制件；然后采用液相浸渍-碳化热压成形或用化学气相沉积增密到所需密度，再高温处理，石英纤维与基体炭间的界面层部分或全部转化成碳化硅。所得石英纤维/炭纤维增强炭基复合材料平板强度较高，弯曲强度达到120～130MPa，上下表面由石英纤维+碳化硅界面层+基体炭组成，可以有效降低平板表面层与硅蒸气反应速度和反应程度，提高平板的使用寿命，相较于普通炭/炭复合材料平板使用寿命提升20％以上，适合高效单晶炉保温盖板和类单晶铸锭炉的盖板、顶板及坩埚护板等。
具体实施方式
实施例1
一种石英纤维/炭纤维增强炭基复合材料平板预制件，该预制件包括：中间层和与所述中间层上下表面通过交替叠加针刺连接的表面层；所述中间层由面密度为280～600g/m2的炭纤维平纹布或斜纹布加面密度为80～120g/m2的短纤维网胎交替叠层针刺而成；所述表面层由面密度180～300g/m2的石英纤维无纬布加面密度为60～120g/m2短石英纤维网胎交替叠加针刺而成。
其中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4，密度0.4～0.6g/cm3。
实施例2
其中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为7∶3，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1，密度0.4～0.6g/cm3。其余同实施例1。
实施例3
一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，包括以下步骤：
将实施例1或实施例2所制得的石英纤维/炭纤维复合预制体，放在合适的不锈钢立方型容器中喷淋或浸渍树脂(酚醛树脂、呋喃树脂或其他残炭率较高的树脂)，然后放在厚度2～8mm不锈钢板上阴干，主要是把多余的树脂流出来，并自然去除一部分挥发物，然后连不锈钢平板和浸渍树脂的预制件推送到平板热压机，垫好限高块，温度控制在150～300℃,待温度升到树脂粘度增大，树脂基本不外流时，加压，压力为50-600t，到厚度后，保压，升温到设定温度200～220℃，保温，2～3小时，然后保压，自然冷却到室温取出，得到第一平板坯,密度为1.3～1.6g/cm3；把第一平板坯放到碳化炉中进行碳化，每块平板坯间垫一层硫酸纸或牛皮纸，每1块～15块平板坯隔一块50～100mm厚的石墨或炭/炭复合材料标准平板，最上面再压一块石墨或炭/炭复合材料标准平板，避免平板坯碳化时变形，得到石英纤维/炭纤维增强炭基平板坯(第二平板坯),密度为1.0～1.3g/cm3；然后把第二平板坯装到加压浸渍炉中浸渍树脂或沥青，再碳化，密度达到1.4～1.6g/cm3，得到第三平板坯；或者采用化学气相沉积增密工艺，把平板预制件装到限域石墨或炭/炭工装中，进行增密，密度达到1.4～1.6g/cm3后，得到石英纤维/炭纤维增强炭基平板坯(第三平板坯)。
然后把所得的石英纤维/炭纤维增强炭基平板坯(第三平板坯)进行表面清理，按碳化装炉方式装入石墨化炉进行高温处理，处理温度为1300～1800℃，保温时间3～15小时，石英纤维表面部分转化成碳化硅；得到石英纤维/炭纤维增强炭基复合材料平板，平板的弯曲强度达到120～130MPa。最后按要求加工到尺寸。所得石英纤维/炭纤维增强炭基复合材料平板上下表面由石英纤维+碳化硅界面层+基体炭组成，可以有效降低平板表面层与硅蒸气反应速度和反应程度，相对于普通炭/炭纤维复合平板的使用寿命提升20％以上，可适用于高效单晶炉保温盖板和类单晶铸锭炉的盖板、顶板及坩埚护板等。
对比例1
其中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4，密度0.4～0.6g/cm3。其余同实施例1。
制备方法同实施例3。
所得平板的弯曲强度为88MPa。使用寿命相较于本发明实施例3的平板降低了30％。
对比例2
其中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1，密度0.5～0.8g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为10∶1，密度0.4～0.6g/cm3。其余同实施例1。
制备方法同实施例3。
所得平板的弯曲强度为92MPa。使用寿命相较于对比例1提高15％。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (7)

1.一种石英纤维/炭纤维增强炭基复合材料平板预制件，其特征在于，包括：中间层和与所述中间层上下表面通过交替叠加针刺连接的表面层；所述中间层由面密度为280~600g/m2的炭纤维平纹布或斜纹布加面密度为80~120 g/m2的短纤维网胎交替叠层针刺而成；所述表面层由面密度180~300 g/m2的石英纤维无纬布加面密度为60~120 g/m2短石英纤维网胎交替叠加针刺而成；所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1~7∶3，密度0.5~0.8 g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4~9∶1，密度0.4~0.6 g/cm3。
2.一种石英纤维/炭纤维增强炭基复合材料平板，其特征在于，使用如权利要求1所述的预制件制得。
3.一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，其特征在于，包括以下步骤：
S1、预制件的制备：按重量比将面密度为280~600 g/m2的炭纤维平纹布或斜纹布加面密度为80~120 g/m2的短纤维网胎交替叠层针刺而得到中间层；在中间层表面由面密度180~300 g/m2的石英纤维无纬布加面密度为60~120 g/m2短石英纤维网胎按重量比交叠层针刺成表面层；翻转后，在中间层另一表面由面密度180~300 g/m2的石英纤维无纬布加面密度为60~120 g/m2短石英纤维网胎按重量比交叠层针刺成另一表面层，得到预制件；
S2、预制件的热压成型：将步骤S1得到的预制件喷淋或浸渍树脂，置于不锈钢板上阴干，将不锈钢板和预制件推送至平板热压机热压成型，冷却至室温，得到密度为1.3~1.6 g/cm3的第一平板坯；
S3、碳化：将步骤S2制得的第一平板坯放入碳化炉中碳化，每块平板坯间垫一层硫酸纸或牛皮纸，每1块~15块平板坯隔一块50~100 mm厚的石墨或炭/炭复合材料标准平板，最上面再压一块石墨或炭/炭复合材料标准平板，避免碳化时变形，得到密度为1.0~1.3 g/cm3的第二平板坯；将第二平板坯通过浸渍树脂或沥青，再碳化，得到密度为1.4~1.6 g/cm3的第三平板坯；
S4、石墨化：将表面清理后的第三平板坯装入石墨化炉进行高温处理，每块平板坯间垫一层硫酸纸或牛皮纸，每1块~15块平板坯隔一块50~100mm厚的石墨或炭/炭复合材料标准平板，最上面再压一块石墨或炭/炭复合材料标准平板，避免石墨化时变形，得到石英纤维表面部分转化为碳化硅的石英纤维/炭纤维增强炭基复合材料平板；所述高温处理的温度为1300~1800℃，时间为3~15小时。
4.根据权利要求3所述的一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，其特征在于，步骤S1中，所述中间层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为9∶1~7∶3，密度0.5~0.8 g/cm3；所述表面层的炭纤维平纹布或斜纹布与短纤维网胎的重量比为6∶4~9∶1，密度0.4~0.6 g/cm3。
5.根据权利要求3所述的一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，其特征在于，步骤S2中，所述树脂包括酚醛树脂或呋喃树脂中的任意一种。
6.根据权利要求3所述的一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，其特征在于，步骤S2中，所述热压成型具体为：将不锈钢平板和浸渍树脂的预制件推送到平板热压机，垫好限高块，温度控制在150~300℃，待温度升到树脂粘度增大，树脂不外流时，加压，压力为20~600 t，与限高块等高时，保压，升温到设定温度200~220℃，保温，2~3小时，继续保压，自然冷却到室温。
7.根据权利要求3所述的一种石英纤维/炭纤维增强炭基复合材料平板的制备方法，其特征在于，步骤S3中，所述第二平板坯还可通过化学气相沉积增密工艺而得到第三平板坯。
CN202111563860.2A 2021-12-20 2021-12-20 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法 Active CN114014678B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111563860.2A CN114014678B (zh) 2021-12-20 2021-12-20 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111563860.2A CN114014678B (zh) 2021-12-20 2021-12-20 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法

Publications (2)

Publication Number Publication Date
CN114014678A CN114014678A (zh) 2022-02-08
CN114014678B true CN114014678B (zh) 2023-02-03

Family

ID=80069345

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111563860.2A Active CN114014678B (zh) 2021-12-20 2021-12-20 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法

Country Status (1)

Country Link
CN (1) CN114014678B (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115385710B (zh) * 2022-09-05 2023-11-03 华东理工大学 一种混编纤维增强的多孔碳基复合材料及其制备方法
CN116462525B (zh) * 2023-06-19 2023-09-05 中国人民解放军国防科技大学 一种连续碳纤维增强超高温陶瓷基复合材料及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1225953A (zh) * 1998-01-19 1999-08-18 住友电气工业株式会社 制造碳化硅单晶的方法和用于制造碳化硅单晶的装置
CN105742810A (zh) * 2016-01-26 2016-07-06 湖北三江航天江北机械工程有限公司 超高温陶瓷基复合材料烧蚀头天线罩罩体的制造方法
CN109721377A (zh) * 2019-01-30 2019-05-07 湖南兴晟新材料科技有限公司 碳纤维增强碳化硅陶瓷基复合材料及其制备方法
CN111848201A (zh) * 2020-07-24 2020-10-30 西安超码科技有限公司 一种具有碳化硅/硅涂层的炭/炭坩埚及其制备方法
CN213142285U (zh) * 2020-09-08 2021-05-07 汨罗市福缘新材料有限公司 一种石墨坩埚盖板

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1225953A (zh) * 1998-01-19 1999-08-18 住友电气工业株式会社 制造碳化硅单晶的方法和用于制造碳化硅单晶的装置
CN105742810A (zh) * 2016-01-26 2016-07-06 湖北三江航天江北机械工程有限公司 超高温陶瓷基复合材料烧蚀头天线罩罩体的制造方法
CN109721377A (zh) * 2019-01-30 2019-05-07 湖南兴晟新材料科技有限公司 碳纤维增强碳化硅陶瓷基复合材料及其制备方法
CN111848201A (zh) * 2020-07-24 2020-10-30 西安超码科技有限公司 一种具有碳化硅/硅涂层的炭/炭坩埚及其制备方法
CN213142285U (zh) * 2020-09-08 2021-05-07 汨罗市福缘新材料有限公司 一种石墨坩埚盖板

Also Published As

Publication number Publication date
CN114014678A (zh) 2022-02-08

Similar Documents

Publication Publication Date Title
CN114014678B (zh) 一种石英纤维/炭纤维增强炭基复合材料平板及其制备方法
EP2093453B1 (en) CVI followed by coal tar pitch densification by VPI
CN107266075B (zh) 一种C/C-SiC复合材料及其制备方法和应用
CN100501185C (zh) 一种高速列车碳/碳制动材料的制备方法
US7927523B2 (en) Densification of C-C composites with pitches followed by CVI/CVD
JP2007535461A (ja) 炭素繊維強化のセラミックの複合体の製造方法
CN113072387A (zh) 一种碳纤维缠绕坩埚及其制备方法
US6261692B1 (en) Carbon-carbon composites containing ceramic power and method for preparing the same
CN106145989A (zh) 一种多晶铸锭炉热场用盖板的制备方法
CN101687715B (zh) 刹车和离合器片的改进
CN114645449A (zh) 一种聚酰亚胺树脂碳改性C/C-SiC摩擦材料的制备方法
CN112266259B (zh) 一种陶瓷基复合材料及其制备方法和应用
JP2005536420A (ja) カーボンハニカム体
CN114368976B (zh) 石英纤维增强炭-二氧化硅复合材料坩埚及其制备方法
CN114014676B (zh) 一种石英纤维/炭纤维增强炭基复合材料保温桶及其制备方法
CN114411242B (zh) 石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法
CN113896560A (zh) 一种工业炉用低密度多孔保温材料的制备方法
CN114014677B (zh) 一种石英纤维/炭纤维增强炭基复合材料坩埚及其制备方法
CN114232074B (zh) 一种石英纤维/炭纤维增强炭基复合材料导流筒及其制备方法
JP3853035B2 (ja) 耐酸化性ｃ／ｃ複合材及びその製造方法
JPH05306180A (ja) 炭素繊維強化炭素−無機化合物複合材料の製造方法
JP3461424B2 (ja) 耐酸化性ｃ／ｃ複合材の製造方法
CN117534494A (zh) 一种航空碳陶刹车材料及其制备方法
JPH0952777A (ja) 耐酸化性ｃ／ｃ複合材の製造方法
JPH08169786A (ja) 耐酸化性炭素繊維強化炭素複合材の製造法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant