CN114411242A - 石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法 - Google Patents

石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法 Download PDF

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CN114411242A
CN114411242A CN202210118258.6A CN202210118258A CN114411242A CN 114411242 A CN114411242 A CN 114411242A CN 202210118258 A CN202210118258 A CN 202210118258A CN 114411242 A CN114411242 A CN 114411242A
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quartz fiber
guide cylinder
fiber reinforced
reinforced carbon
composite material
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CN114411242B (zh
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陈腾飞
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Central South University
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Abstract

本发明涉及石英纤维增强炭‑二氧化硅复合材料导流筒及其制备方法，属于石英纤维及炭基复合材料制备技术领域。采用由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～150g/m2短石英纤维网胎交叠层针刺得密度为0.35～0.7g/cm3的石英纤维预制件，然后经固化定型、增密至1.0～1.3g/cm3后，进行第一次高温处理，机加至设计尺寸；加压浸渍硅溶胶，干燥‑固化‑烧结，必要时重复这一程序，进行第二次高温处理，表面抛光，得到密度为1.4～1.8g/cm3的石英纤维增强炭‑二氧化硅复合材料导流筒。提高导流筒的使用寿命。

Description

石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法
技术领域
本发明涉及石英纤维及炭基复合材料制备技术领域，具体涉及石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法。
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的热场部件上的应用非常广泛，其中，炭/炭复合材料导流筒是单晶炉热场系统的关键部件之一。
在单晶硅拉制时，热场部件处于硅蒸气和惰性气体的混合气氛中，硅蒸气会在热场部件表面沉积并部分与炭/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。而且在单晶拉制时，单晶硅棒会穿过导流筒，由于导流筒的下口与硅棒外径间距很小，穿过导流筒的那段硅棒一般碳含量偏高，从而影响这段硅棒做成硅片的质量，因而有些厂家在炭/炭或石墨导流筒的表面做碳化硅涂层，由于碳化硅与炭/炭或石墨的热膨胀系数不匹配，使用一段时间后，碳化硅涂层容易分层或脱落，从而影响继续使用；有些厂家使用石英导流筒，但石英在高温下容易软化，给使用带来风险。
发明内容
针对现有单晶炉用炭/炭复合材料或石墨导流筒容易受硅蒸气硅化影响和穿过导流筒的那段硅棒碳含量偏高的问题，本发明提供石英纤维增强炭-二氧化硅复合材料导流筒及其制备方法，采用石英纤维制备预制件，通过化学气相沉积(渗透)和(或)加压浸渍树脂或沥青-碳化工艺增密，然后高温处理使得石英纤维与基体炭间形成碳化硅界面层，再机加工，得到石英纤维增强炭基复合材料导流筒坯；然后加压浸渍硅溶胶进入石英纤维增强炭基复合材料导流筒坯，经干燥-固化-烧结，再进行最后高温处理，表面打磨-抛光，得到石英纤维增强炭-二氧化硅复合材料导流筒。从而使得导流筒本体及表面与硅蒸气基本不反应，并降低表面的碳、氧含量。
本发明提供一种石英纤维导流筒预制件，该预制件由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～150g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为5∶5～9∶1，密度为0.35～0.7g/cm3。
本发明还提供了一种石英纤维增强炭-二氧化硅复合材料导流筒，采用上述的石英纤维导流筒预制件经固化定型、化学气相沉积增密或树脂或沥青浸渍-碳化增密至1.0～1.3g/cm3后，进行第一次高温处理，机加至设计尺寸；加压浸渍硅溶胶，经干燥-固化-烧结，密度达到1.4～1.8g/cm3以上，再进行第二次高温处理，表面打磨-抛光，即得。
优选地，固化定型的温度为150～300℃。
优选地，第一次高温处理的温度为1300～1900℃，保温时间为2～20h。
优选地，所述硅溶胶的质量分数为10～45％。
优选地，第二次高温处理的温度为1300～1900℃，保温时间为2～10h。
进一步地，本发明还提供了上述的石英纤维增强炭-二氧化硅复合材料导流筒的制备方法，包括以下步骤：
S1、由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～150g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为5∶5～9∶1，得到密度为0.35～0.7g/cm3的石英纤维导流筒预制件；
S2、把所制得的石英纤维导流筒预制体套在合适的钢模或石墨模具上，使导流筒预制件的内表面与模具的外形面贴合良好，然后喷淋或浸渍树脂或有机粘结剂，放置1～10小时，在导流筒外表面套上外钢模，外钢模的内型面与导流筒预制件的外形面贴合紧密，并使预制件的外径与导流筒产品的外径大1～2mm，然后固定好外模；然后把套好的预制件(带模具)送入烘箱中固化定型，温度控制在150～300℃，待烘箱不往外冒烟时，保温1～10小时，降温，脱模，得到定型的石英纤维预制体；然后采用化学气相沉积增密工艺或树脂或沥青浸渍-碳化增密工艺，把预制件增密到1.0～1.3g/cm3后，进行高温处理，处理温度为1300～1900℃，保温时间2～20小时，石英纤维与基体炭界面部分或全部转化成碳化硅，然后机加到产品尺寸，得到石英纤维增强炭基复合材料导流筒坯；
S3、采用加压浸渍工艺将硅溶胶浸渍进入石英纤维增强炭基复合材料导流筒坯，然后干燥-固化-烧结，必要时重复这一程序，使得密度达到1.4～1.8g/cm3后，进行最后高温处理，处理温度为1300～1900℃，保温时间2～10小时，导流筒表面打磨-抛光处理，得到石英纤维增强炭-二氧化硅复合材料导流筒。
优选地，步骤S1中，所述树脂为酚醛树脂、呋喃树脂或其他残炭率较高的树脂。
优选地，步骤S2中，所述外钢模分为3-6瓣。
本发明技术方案，具有如下优点：
本发明提供的一种石英纤维增强炭-二氧化硅复合材料导流筒，其预制件由石英纤维无纬布或平纹布+短石英纤维网胎交替叠层针刺而成；石英纤维布和短石英纤维网胎交替叠层针刺得到的预制件具有较多的孔隙，通过对石英纤维布和短石英纤维网胎的面密度及布网重量比和最终的密度进行控制，可实现其孔隙大小的控制，有利于在化学沉积增密时控制石英纤维增强炭基复合材料导流筒坯及最终产品的密度。预制件经套模固化定型，再用化学气相沉积增密或液相浸渍-碳化增密到所需密度，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。然后机械加工，再加压浸渍硅溶胶干燥固化-烧结，最后高温处理，使炭基体与二氧化硅间的界面部分或全部转化成碳化硅，提高界面结合强度；而且由于采用内外模具进行固化定型，导流筒内、外型面加工量减少，导流筒的纤维体积含量增加，所得石英纤维增强炭-二氧化硅复合材料导流筒强度高，孔隙率低，相对于普通炭/炭复合材料导流筒的使用寿命提升50％以上；而且该工艺制备的石英纤维增强炭-二氧化硅复合材料导流筒，主要成分为石英纤维和二氧化硅、碳化硅、基体炭，基体炭的含量显著降低，而且周围是石英或二氧化硅，可以显著降低拉晶气氛的碳含量，适合制备高效单晶炉的热场部件。
具体实施方式
支持权利要求书中限定的每一个技术方案。
实施例1
一种石英纤维导流筒预制件，该预制件由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～120g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为5∶5，密度为0.35g/cm3。
实施例2
一种石英纤维导流筒预制件，该预制件由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～120g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为9∶1，密度为0.7g/cm3。
实施例3
一种石英纤维增强炭-二氧化硅复合材料导流筒的制备方法，包括以下步骤：
S1、将实施例1所制得的石英纤维导流筒预制体套在合适的钢模或石墨模具上，使导流筒预制件的内表面与模具的外形面贴合良好，然后喷淋或浸渍树脂或有机粘结剂，放置1～10小时，在导流筒外表面套上外钢模，外钢模的内型面与导流筒预制件的外形面贴合紧密，并使预制件的外径与导流筒产品的外径大1～2mm，然后固定好外模；然后把套好的预制件(带模具)送入烘箱中固化定型，温度控制在150～300℃，待烘箱不往外冒烟时，保温1～10小时，降温，脱模，得到定型的石英纤维预制体；然后采用化学气相沉积增密工艺或树脂或沥青浸渍-碳化增密工艺，把预制件增密到1.0g/cm3后，进行第一次高温处理，处理温度为1300～1900℃，保温时间2～20小时，石英纤维与基体炭界面部分或全部转化成碳化硅，然后机加到产品尺寸，得到石英纤维增强炭基复合材料导流筒坯；
S2、采用加压浸渍工艺将硅溶胶浸渍进入石英纤维增强炭基复合材料导流筒坯硅溶胶，然后干燥-固化-烧结，使得密度达到1.4g/cm3后，进行第二次高温处理，处理温度为1300～1900℃，保温时间2～10小时，导流筒表面打磨-抛光处理，得到石英纤维增强炭-二氧化硅复合材料导流筒。
其中，步骤S1中，所述树脂为酚醛树脂、呋喃树脂或其他残炭率较高的树脂。
其中，步骤S2中，所述外钢模分为3-6瓣。
实施例4
一种石英纤维增强炭-二氧化硅复合材料导流筒的制备方法，包括以下步骤：
S1、将实施例2所制得的石英纤维导流筒预制体套在合适的钢模或石墨模具上，使导流筒预制件的内表面与模具的外形面贴合良好，然后喷淋或浸渍树脂或有机粘结剂，放置1～10小时，在导流筒外表面套上外钢模，外钢模的内型面与导流筒预制件的外形面贴合紧密，并使预制件的外径与导流筒产品的外径大1～2mm，然后固定好外模；然后把套好的预制件(带模具)送入烘箱中固化定型，温度控制在150～300℃，待烘箱不往外冒烟时，保温1～10小时，降温，脱模，得到定型的石英纤维预制体；然后采用化学气相沉积增密工艺或树脂或沥青浸渍-碳化增密工艺，把预制件增密到1.3g/cm3后，进行第一次高温处理，处理温度为1300～1900℃，保温时间2～20小时，石英纤维与基体炭界面部分或全部转化成碳化硅，然后机加到产品尺寸，得到石英纤维增强炭基复合材料导流筒坯；
S2、采用加压浸渍工艺将硅溶胶浸渍进入石英纤维增强炭基复合材料导流筒坯硅溶胶，然后干燥-固化-烧结，重复加压浸渍、干燥-固化-烧结，使得密度达到1.8g/cm3后，进行第二次高温处理，处理温度为1300～1900℃，保温时间2～10小时，导流筒表面打磨-抛光处理，得到石英纤维增强炭-二氧化硅复合材料导流筒。
其中，步骤S1中，所述树脂为酚醛树脂、呋喃树脂或其他残炭率较高的树脂。
其中，步骤S2中，所述外钢模分为3-6瓣。
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 (8)

1.一种石英纤维导流筒预制件，其特征在于，该预制件由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～150g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为5∶5～9∶1，密度为0.35～0.7g/cm3。
2.一种石英纤维增强炭-二氧化硅复合材料导流筒，其特征在于，采用如权利要求1所述的石英纤维导流筒预制件经固化定型、化学气相沉积增密或树脂或沥青浸渍-碳化增密至1.0～1.3g/cm3后，进行第一次高温处理，机加至设计尺寸；加压浸渍硅溶胶，干燥-固化-烧结，密度达到1.4～1.8g/cm3以上，进行第二次高温处理，表面抛光，即得。
3.根据权利要求2所述的石英纤维增强炭-二氧化硅复合材料导流筒，其特征在于，固化定型的温度为150～300℃。
4.根据权利要求2所述的石英纤维增强炭-二氧化硅复合材料导流筒，其特征在于，第一次高温处理的温度为1300～1900℃，保温时间为2～20h。
5.根据权利要求2所述的石英纤维增强炭-二氧化硅复合材料导流筒，其特征在于，所述硅溶胶的质量分数为10～45％。
6.根据权利要求2所述的石英纤维增强炭-二氧化硅复合材料导流筒，其特征在于，第二次高温处理的温度为1300～1900℃，保温时间为2～10h。
7.根据权利要求2-6任一项所述的石英纤维增强炭-二氧化硅复合材料导流筒的制备方法，其特征在于，包括以下步骤：
S1、由面密度180～600g/m2的石英纤维无纬布或平纹布加面密度为30～150g/m2短石英纤维网胎交叠层针刺而成，布∶网重量比为5∶5～9∶1，得到密度为0.35～0.7g/cm3的石英纤维导流筒预制件；
S2、把所制得的石英纤维导流筒预制体套在合适的钢模或石墨模具上，使导流筒预制件的内表面与模具的外形面贴合良好，然后喷淋或浸渍树脂或有机粘结剂，放置1～10小时，在导流筒外表面套上外钢模，外钢模的内型面与导流筒预制件的外形面贴合紧密，并使预制件的外径与导流筒产品的外径大1～2mm，然后固定好外模；然后把套好的预制件送入烘箱中固化定型，温度控制在150～300℃，待烘箱不往外冒烟时，保温1～10小时，降温，脱模，得到定型的石英纤维预制体；然后采用化学气相沉积增密工艺和(或)树脂或沥青浸渍-碳化增密工艺，把预制件增密到1.0～1.3g/cm3后，进行高温处理，处理温度为1300～1900℃，保温时间2～20小时，石英纤维与基体炭界面部分或全部转化成碳化硅，然后机加到产品尺寸，得到石英纤维增强炭基复合材料导流筒坯；
S3、采用加压浸渍工艺将硅溶胶浸渍进入石英纤维增强炭基复合材料导流筒坯，然后干燥-固化-烧结，使得密度达到1.4～1.8g/cm3后，进行最后高温处理，处理温度为1300～1900℃，保温时间2～10小时，导流筒表面打磨-抛光处理，得到石英纤维增强炭-二氧化硅复合材料导流筒。
8.根据权利要求7所述的石英纤维增强炭-二氧化硅复合材料导流筒的制备方法，其特征在于，步骤S1中，所述树脂为酚醛树脂、呋喃树脂或其他残炭率较高的树脂。
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