CN108069724A - 一种制备C/SiC复合材料的方法 - Google Patents
一种制备C/SiC复合材料的方法 Download PDFInfo
- Publication number
- CN108069724A CN108069724A CN201611020022.XA CN201611020022A CN108069724A CN 108069724 A CN108069724 A CN 108069724A CN 201611020022 A CN201611020022 A CN 201611020022A CN 108069724 A CN108069724 A CN 108069724A
- Authority
- CN
- China
- Prior art keywords
- composite materials
- preparing
- temperature
- infiltration
- hybrid resin
- 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.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 title claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 53
- 239000011347 resin Substances 0.000 claims abstract description 53
- 230000008595 infiltration Effects 0.000 claims abstract description 45
- 238000001764 infiltration Methods 0.000 claims abstract description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000013312 flour Nutrition 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000003822 epoxy resin Substances 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 23
- 238000004321 preservation Methods 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- -1 ammonia phenolic aldehyde Chemical class 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 239000004744 fabric Substances 0.000 abstract description 6
- 238000007747 plating Methods 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/521—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained by impregnation of carbon products with a carbonisable material
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
本发明提出一种制备C/SiC复合材料的方法,通过制备C/C复合材料、混合树脂配制、混合树脂涂抹在C/C复合材料表面、预固化、高温熔渗等步骤得到C/SiC复合材料。本发明通过配制混合树脂,硅粉能容易地布置在所需熔渗的构件部位,解决RMI工艺制备复杂形状C/SiC材料均匀布硅的难题,可有效调节熔渗反应,得到反应均衡的C/SiC复合材料,适宜制备大尺寸构件。
Description
技术领域
本发明涉及一种制备C/SiC复合材料的方法,属于复合材料制备技术领域。
背景技术
C/SiC复合材料的密度只有1.8~2.5g/cm3,但在高温环境下却有着相当高的断裂强度和韧性,具有密度低、高温强度高、高温抗氧化和韧性断裂等优点,是高超声速飞行器前缘、前体舱、燃烧室和翼舵等热结构件的重要候选材料。
C/SiC复合材料的制备技术主要有化学气相渗透CVI、浸渍裂解PIP以及反应熔渗RMI技术。前两种工艺存在致密化速度低、生产周期长、制备成本高、致密度及气孔率等性能不能满足需求等问题。相比而言,反应熔渗RMI制备技术则具有成本低、周期短,制备的复合材料致密化程度高等优点。因此,国外较为重视熔渗技术的研究,美国X-38再入飞行器的C/SiC鼻锥即采用反应熔渗技术制备,并通过了再入飞行验证。
反应溶渗法(RMI)的基本原理是将熔渗金属加热到熔融液态,然后在一定的压力或无压条件下利用毛细作用渗入到预制体内部,发生化学反应后生成所需产物以制备得到复合材料。
目前反应溶渗法制备C/SiC复合材料时大多采用将熔渗原料铺在坩锅底部,待熔渗制品直接放置在熔渗原料上面,待熔渗原料熔融后通过毛细作用来渗入构件内部,与基体碳发生反应制得C/SiC复合材料。因毛细渗透作用的深度局限,此方法只适用于小尺寸或高度较低的构件,大尺寸构件常常需仿形工装在多部位布熔渗原料,但成本较高且存在分布不均匀的问题。
发明内容
本发明的目的在于克服现有技术不足,提供一种工艺可控、操作简便、熔渗原料分布均匀、反应稳定的制备C/SiC复合材料的方法。
本发明的技术解决方案:一种制备C/SiC复合材料的方法,通过以下步骤实现:
第一步,制备C/C复合材料,
本步骤C/C复合材料的密度不能过高,密度优选在1.2~1.6g/cm3。
C/C复合材料可以采用公知技术进行制备,可以为化学气相沉积、前驱体碳化处理等工艺制备。
进一步,本发明同时提供了一种更优选的C/C复合材料制备方法,具体如下:
A1.1、在纤维预制体表面制备一层热解碳(PyC)界面层;
A1.2、在惰性气氛、1700℃~1900℃条件下,进行2~4小时的高温处理;
A1.3、采用氨酚醛先驱体浸渍剂,进行真空浸渍-压力固化-高温裂解,制备C/C复合材料;
A1.4、重复步骤A1.3直至复合材料密度为1.2g/cm3~1.6g/cm3。
采用本优选方式制备的C/C复合材料中基体C尺寸较小,比表面积大,容易与熔融硅发生反应。
复合材料密度低于1.2g/cm3时,孔隙率较大,为后续渗硅提供了足够的反应熔渗空间,但获得的材料力学性能较差;复合材料密度高于1.6g/cm3时,孔隙率较小,不利于后续渗硅处理。当复合材料密度在上述范围内变化,对材料力学性能及后续渗硅处理影响不明显。
第二步、混合树脂配制,
将硅粉与环氧树脂体系(含固化剂)均匀混合制成混合树脂,所述的混合树脂的邵氏硬度为HA10~HA30;
若环氧树脂体系含量过小,混合树脂黏性差,硬度偏大,其树脂不能很好的附着在构件表面,因此,环氧树脂含量不能低于5%;若环氧树脂含量过高,硬度偏小,混合树脂在构件预固化阶段发生软化流动,硅粉可能出现局部堆积或缺料的不均匀问题,因此,环氧树脂含量不能高于30%。混合树脂的硬度在上述范围内变化,对后续熔渗反应影响不明显。
混合树脂配制时可以添加适量有机溶剂调节粘度,但要保证环氧树脂所占的质量百分比不能超出5%~30%,本领域技术人员根据实际采用的环氧树脂种类和硅粉,保证混合后的树脂邵氏硬度在上述要求范围内即可。
本发明使用的Si粉为微纳米级,采用市售产品。本发明对环氧树脂种类没有特殊限制,如常用的双酚A型环氧树脂,间苯二酚型环氧树脂,溴化双酚A型环氧树脂和酚醛型环氧树脂。
本发明中环氧树脂体系高温裂解为多孔碳网络结构,在后续熔渗反应中会碳化,碳化后与制备的C/SiC复合材料易于分离。
第三步,将第二步制备得到的混合树脂涂抹在第一步得到的C/C复合材料所需熔渗表面,并压实;
混合树脂涂抹的厚度根据该部位体积、密度及所需熔渗的原料质量来计算,保证构件反应后既不缺料也无过多残余熔渗原料,一般控制在复合材料厚度的0.2~1.0倍范围内。
本发明由于在第二步中要求了树脂特性,约束了混合树脂的硬度,保证了在此步骤中混合树脂能轻松粘接于需要反应熔渗的构件部位表面,同时在一定时间内不会软化变形。
第四步,预固化,
将第三步得到的C/C复合材料在预固化温度TYG下,保温不低于0.5小时,不高于2小时,TYG的取值范围为TJ~TJ+50℃,TJ为环氧树脂交联固化的开始温度;
本步骤预固化,使树脂初步形成三维网络结构,混合树脂与构件形成一整体,使其在后续高温时树脂无软化剥离现象,保证了后续渗硅的顺利进行。由于环氧树脂体系为室温固化体系,混合树脂在涂抹到C/C复合材料材料表面时可以在室温下放置一段时间,使其能初步形成三维网络结构,避免在后续高温熔渗时,环氧树脂粘度急剧降低,使混合树脂无法完好地附着在构件表面,熔渗反应无法进行,若TYG取值太高或保温时间过长,环氧树脂固化程度过高,树脂完全硬化,降温后与基体界面会产生一定应力,大尺寸构件在后续熔渗工序装炉搬运时有剥落的隐患。在上述要求范围内变化,对后续熔渗反应没有明显影响。本领域技术人员根据实际生产在上述范围内选择合适的温度和保温时间。
第五步,高温熔渗,得到C/SiC复合材料。
高温熔渗反应为本领域公知技术,本领域技术人员根据具体生产实际确定最佳熔渗工艺温度和工艺。
进一步,本发明提供了一种更优选的熔渗工艺,具体如下:
A5.1、熔渗前高温处理,
经预固化的C/C复合材料在惰性气氛中升温至硅的熔融温度以下20~70℃,保温0.5~1小时;
本步骤中在硅的熔融温度以下20~70℃保温0.5~1小时的作用是将硅粉升温至临近熔化状态,设置保温为了保证构件的温度均匀。不仅避免硅粉在高温熔渗前提前汽化导致的损耗,而且大尺寸构件温度均匀也利于消除升温中产生的应力集中问题。在上述要求范围内变化,对后续熔渗反应没有明显影响。
本领域技术人员根据实际生产在上述范围内选择合适的温度和保温时间。本步骤对升温速率无特殊要求,依据设备能力及构件结构特性决定,以控制构件不产生应力变形为要素。
A5.2、将步骤A5.1熔渗前高温处理的复合材料,继续加热升温至熔渗温度,保温,完成高温熔渗反应,得到C/SiC复合材料。
本步骤快速升温至最佳熔渗工艺温度,可以减少熔渗原料熔融初期粘度较大对工艺带来的不利影响。具体升温速率依据设备能力及构件结构特性决定,尽量控制在1个小时内完成升温。
本发明与现有技术相比的有益效果:
(1)本发明通过配制混合树脂,硅粉能容易地布置在所需熔渗的构件部位,解决RMI工艺制备复杂形状C/SiC材料均匀布硅的难题,可有效调节熔渗反应,得到反应均衡的C/SiC复合材料,适宜制备大尺寸构件;
(2)本发明克服了反应熔渗后构件表面容易粘附大量未反应硅的缺点,环氧树脂形成的网状结构使得熔融硅不易在构件表面聚集,且构件表面容易清理;
(3)本发明适宜制备异形构件,解决大尺寸构件无支撑下斜面等部位无法布置硅粉的难题,避免了现有技术中制备大尺寸异形构件时需多次渗硅的问题;
(4)本发明可针对不同部位熔渗所需的硅粉数量进行调节,适用于变厚度构件的均匀渗硅;
(5)本发明不需加工熔渗坩埚及布料仿形工装,可极大降低成本;
(6)本发明通过对混合树脂配制、预固化处理、渗硅前高温处理等步骤工艺设计,保证了熔渗反应的进行。
附图说明
图1为本发明流程图。
具体实施方式
下面结合具体实例及附图对本发明进行详细说明。
实施例1
制备工艺如图1所示,将碳纤维缝合预制体(具有波纹结构)装入CVI-C炉内,在真空和1020℃条件下,通入C3H8与Ar混合气体,沉积180小时出炉。经过1700℃高温处理,采用氨酚醛先驱体浸渍剂,进行真空浸渍-压力固化-800℃高温裂解,制备出密度为1.40g/cm3的C/C波纹板。采用硅粉与环氧树脂(含固化剂)质量比为3:1的比例均匀搅拌制成混合树脂,得到硬度约为HA13的混合树脂(该状态树脂含量约25%),混合树脂均匀的涂覆到C/C波纹板的各个表面上,其中涂覆的混合树脂厚度约为波纹板该处厚度的0.7倍左右,将涂覆有混合树脂的C/C波纹板在30℃下放置1小时,在抽真空加热至1400℃保温30min,随后在1小时内升至1750℃,并保温90min,制备出C/SiC波纹复合材料,密度为2.2g/cm3,弯曲强度为289MPa。
实施例2
采用与实施例1相同的工艺,改变氨酚醛浸渍裂解次数,制备出密度为1.20g/cm3的C/C波纹板。采用硅粉与环氧树脂(含固化剂)质量比为3:1的比例均匀搅拌制成混合树脂,得到硬度约为HA13的混合树脂(该状态树脂含量25%),混合树脂均匀的涂覆到C/C波纹板的各个表面上,其中涂覆的混合树脂厚度约为波纹板该处厚度的0.7倍左右,将涂覆有混合树脂的C/C波纹板在30℃下放置1小时,在抽真空加热至1400℃保温30min,随后在1小时内升至1750℃,并保温90min,制备出C/SiC波纹板,密度为2.0g/cm3,弯曲强度为198MPa。
实施例3
采用与实施例1相同的工艺,制备出密度为1.40g/cm3的C/C波纹板。采用硅粉与环氧树脂(含固化剂)质量比为5:1的比例均匀搅拌制成混合树脂,得到硬度约为HA24的混合树脂(该状态树脂含量约16%),混合树脂均匀的涂覆到C/C波纹板的各个表面上,其中涂覆的混合树脂厚度约为波纹板该处厚度的0.6倍左右,将涂覆有混合树脂的C/C波纹板在30℃下放置1小时,在抽真空加热至1400℃保温30min,随后在1小时内升至1750℃,并保温90min,制备出C/SiC波纹板,密度为2.1g/cm3,弯曲强度为254MPa。
实施例4
采用常规方式制备出密度为1.30g/cm3的C/C波纹板。在环氧树脂(含固化剂)按1:8的质量比加入到200目的硅粉中搅拌均匀,30℃放置一段时间,得到硬度约为HA25的混合树脂(该状态树脂含量约8.9%)混合树脂。将均匀的涂覆到C/C波纹板的各个表面上,其中涂覆的混合树脂厚度约为波纹板该处厚度的0.5倍左右,将涂覆有混合树脂的C/C波纹板在室温下放置1小时,在抽真空加热至1400℃保温30min,随后在1小时内升至1750℃,并保温90min,制备出C/SiC波纹板,密度为2.1g/cm3,弯曲强度为249MPa。
本发明未详细说明部分为本领域技术人员公知技术。
Claims (7)
1.一种制备C/SiC复合材料的方法,其特征在于,通过以下步骤实现:
第一步,制备C/C复合材料;
第二步,混合树脂配制,
将硅粉与环氧树脂体系均匀混合制成混合树脂,所述的混合树脂的邵氏硬度为HA10~HA30;
第三步,将第二步制备得到的混合树脂涂抹在第一步得到的C/C复合材料所需熔渗表面,并压实;
第四步,预固化,
将第三步得到的C/C复合材料在预固化温度TYG下,保温不低于0.5小时,不高于2小时,TYG的取值范围为TJ~TJ+50℃,TJ为环氧树脂交联固化的开始温度;
第五步,高温熔渗,得到C/SiC复合材料。
2.根据权利要求1所述的一种制备C/SiC复合材料的方法,其特征在于:所述第五步熔渗通过以下步骤实现,
A5.1、熔渗前高温处理,
经预固化的C/C复合材料在惰性气氛中升温至硅的熔融温度以下20~70℃,保温0.5~1小时;
A5.2、将步骤A5.1熔渗前高温处理的复合材料,继续加热升温至熔渗温度,保温,完成高温熔渗反应,得到C/SiC复合材料。
3.根据权利要求2所述的一种制备C/SiC复合材料的方法,其特征在于:所述步骤A5.2中1个小时内完成升温至熔渗温度。
4.根据权利要求1所述的一种制备C/SiC复合材料的方法,其特征在于:所述第一步制备C/C复合材料采用如下步骤,
A1.1、在纤维预制体表面制备一层热解碳(PyC)界面层;
A1.2、在惰性气氛、1700℃~1900℃条件下,进行2~4小时的高温处理;
A1.3、采用氨酚醛先驱体浸渍剂,进行真空浸渍-压力固化-高温裂解,制备C/C复合材料;
A1.4、重复步骤A1.3直至复合材料密度为1.2g/cm3~1.6g/cm3。
5.根据权利要求1所述的一种制备C/SiC复合材料的方法,其特征在于:所述第一步中C/C复合材料的密度为1.2~1.6g/cm3。
6.根据权利要求1所述的一种制备C/SiC复合材料的方法,其特征在于:所述第二步中环氧树脂所占的质量百分比为5%~30%。
7.根据权利要求1所述的一种制备C/SiC复合材料的方法,其特征在于:所述第三步中混合树脂涂抹的厚度为复合材料厚度的0.2~1.0倍。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611020022.XA CN108069724B (zh) | 2016-11-18 | 2016-11-18 | 一种制备C/SiC复合材料的方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611020022.XA CN108069724B (zh) | 2016-11-18 | 2016-11-18 | 一种制备C/SiC复合材料的方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108069724A true CN108069724A (zh) | 2018-05-25 |
CN108069724B CN108069724B (zh) | 2021-03-09 |
Family
ID=62160538
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201611020022.XA Active CN108069724B (zh) | 2016-11-18 | 2016-11-18 | 一种制备C/SiC复合材料的方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108069724B (zh) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108706977A (zh) * | 2018-06-04 | 2018-10-26 | 陕西固勤材料技术有限公司 | 一种反应烧结碳化硅的装炉方法 |
CN109293383A (zh) * | 2018-10-31 | 2019-02-01 | 航天特种材料及工艺技术研究所 | 一种纤维增强碳-碳化硅陶瓷基复合材料及其制备方法 |
CN112479719A (zh) * | 2020-11-26 | 2021-03-12 | 航天特种材料及工艺技术研究所 | 一种反应熔渗法制备陶瓷基复合材料的布料方法及其应用 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101693628A (zh) * | 2009-10-20 | 2010-04-14 | 西北工业大学 | 纤维增强ZrC陶瓷基复合材料的制备方法 |
CN104496510A (zh) * | 2014-12-05 | 2015-04-08 | 航天特种材料及工艺技术研究所 | 一种炭/炭复合材料的制备方法 |
CN106507851B (zh) * | 2013-12-25 | 2016-05-11 | 中国科学院上海硅酸盐研究所 | 一种低热膨胀系数的纤维增强陶瓷基复合材料制备方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20020022453A (ko) * | 2000-09-20 | 2002-03-27 | 한종웅 | 원적외선 방사체 조성물 |
-
2016
- 2016-11-18 CN CN201611020022.XA patent/CN108069724B/zh active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101693628A (zh) * | 2009-10-20 | 2010-04-14 | 西北工业大学 | 纤维增强ZrC陶瓷基复合材料的制备方法 |
CN106507851B (zh) * | 2013-12-25 | 2016-05-11 | 中国科学院上海硅酸盐研究所 | 一种低热膨胀系数的纤维增强陶瓷基复合材料制备方法 |
CN104496510A (zh) * | 2014-12-05 | 2015-04-08 | 航天特种材料及工艺技术研究所 | 一种炭/炭复合材料的制备方法 |
Non-Patent Citations (1)
Title |
---|
MIN NIU,HONGJIE WANG,LEI SU,XINGYU FAN,DAHAI ZHANG,JIANJUN SHI: "SiC/(SiC+glass)/glass coating for carbon-bonded carbon fibre composites", 《ROYAL SOCIETY OF CHEMISTRY》 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108706977A (zh) * | 2018-06-04 | 2018-10-26 | 陕西固勤材料技术有限公司 | 一种反应烧结碳化硅的装炉方法 |
CN109293383A (zh) * | 2018-10-31 | 2019-02-01 | 航天特种材料及工艺技术研究所 | 一种纤维增强碳-碳化硅陶瓷基复合材料及其制备方法 |
CN109293383B (zh) * | 2018-10-31 | 2021-06-25 | 航天特种材料及工艺技术研究所 | 一种纤维增强碳-碳化硅陶瓷基复合材料及其制备方法 |
CN112479719A (zh) * | 2020-11-26 | 2021-03-12 | 航天特种材料及工艺技术研究所 | 一种反应熔渗法制备陶瓷基复合材料的布料方法及其应用 |
CN112479719B (zh) * | 2020-11-26 | 2022-04-05 | 航天特种材料及工艺技术研究所 | 一种反应熔渗法制备陶瓷基复合材料的布料方法及其应用 |
Also Published As
Publication number | Publication date |
---|---|
CN108069724B (zh) | 2021-03-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106927846B (zh) | 一种C/C-SiC复合材料零件的制备方法及其产品 | |
CN105218156B (zh) | C/C复合材料表面ZrC‑SiC涂层制备方法 | |
CN110330351B (zh) | 一种SiC纤维增强SiC陶瓷基零件的制备方法及产品 | |
CN102295474B (zh) | 一种SiC-TaC涂层/基体协同改性C/C复合材料制备方法 | |
CN106278278B (zh) | 一种通过修饰前驱体来调控碳化硅热导率的方法 | |
CN109437956A (zh) | 适用于热压法快速制备的碳碳复合材料平板及其制备方法 | |
CN105367106B (zh) | 碳纤维增强碳化锆复合材料及其制备方法 | |
CN104831107B (zh) | 一种耐烧蚀炭/炭‑碳化锆‑铜复合材料及其制备方法 | |
CN108069724A (zh) | 一种制备C/SiC复合材料的方法 | |
CN103992115A (zh) | 一种C/SiC-HfC碳纤维增强超高温陶瓷基复合材料的制备方法 | |
CN109970460A (zh) | 一种碳纤维增强(碳-)碳化硅基-超高温陶瓷基复合材料及其制备方法 | |
CN105016759A (zh) | 一种C/SiC复合材料的快速制备方法 | |
CN103373862B (zh) | 在陶瓷基质复合材料中产生内腔室的方法及用于其的心轴 | |
CN108484173B (zh) | SiCf/SiC复合材料及其制备方法 | |
CN104496507B (zh) | 一种面向燃气轮机热端部件的复杂结构陶瓷零件制造方法 | |
CN105237020B (zh) | 一种碳纤维增强ZrB2-ZrN复相陶瓷基复合材料及其制备方法 | |
CN112409003B (zh) | 一种杂化基体碳化硅基复合材料及其制备方法 | |
CN109592987A (zh) | 一种含富碳氮化硼界面相C/C-SiC复合材料的制备方法 | |
CN104926346B (zh) | 一种含界面相的氧化铝纤维织物增强碳化硅陶瓷及其制备方法 | |
CN108129156A (zh) | 一种碳陶复合材料及其先驱体浸渍制备方法 | |
CN103724033B (zh) | 一种立体织物增强氮化硅-碳化硅陶瓷复合材料及其制备方法 | |
CN106507783B (zh) | 碳/碳化硅陶瓷基复合材料刹车盘的制造方法 | |
CN109851382A (zh) | 一种C/C-TiC陶瓷基复合材料及原位反应法制备该陶瓷基复合材料的方法 | |
CN101348370A (zh) | 一种碳化物陶瓷的先驱体溶液、碳化物陶瓷及制备方法 | |
CN103342573B (zh) | 一种金刚石薄膜增强碳/碳复合材料热导率的方法 |
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 |