CN101550017B - 高温炉用固化碳纤维保温材料及其生产工艺 - Google Patents

高温炉用固化碳纤维保温材料及其生产工艺 Download PDF

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CN101550017B
CN101550017B CN 200910043408 CN200910043408A CN101550017B CN 101550017 B CN101550017 B CN 101550017B CN 200910043408 CN200910043408 CN 200910043408 CN 200910043408 A CN200910043408 A CN 200910043408A CN 101550017 B CN101550017 B CN 101550017B
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carbon fiber
thermal insulating
high temperature
insulating material
temperature furnace
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廖寄乔
邰卫平
王跃军
龚玉良
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Hunan gold carbon Limited by Share Ltd
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HUNAN KBCARBON COMPOSITE SCIENCE AND TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种工艺简单、导热系数小的高温炉用固化碳纤维保温材料及其生产工艺，其特征是它由碳纤维经预制体制备-增密-热振纯化-机加工制成，本发明在预制体制备中无须粘接、浸渍、固化和炭化等过程，其工艺简单且节能环保，预制体内部碳纤维纵横交错，抱合力较强，不会脱层，结构稳定，导热系数≤0.8W/mK，保温性能优良；产品由高强度碳纤维和碳素基质构成，具有高比强度、耐高温、耐腐蚀、保温性能好等优良性能，兼具耐火、保温双重特性，且能承载一定的重荷，是替代高温炉用相关石墨制品及软炭毡的理想的升级产品。

Description

高温炉用固化碳纤维保温材料及其生产工艺
技术领域：
本发明涉及一种高温炉用保温材料，具体地说是一种高温炉用固化碳纤维保温材料及其生产工艺。
背景技术：
单晶炉、多晶硅铸锭炉及粉末冶金烧结炉工作时，炉内温度最高达1600℃以上，为减少热损失，降低能耗，保证炉内温度满足工艺要求，离不开既能耐高温又具有良好保温性能的耐火保温材料作炉衬。目前，如单晶炉其炉衬一般由石墨制品和软炭毡组成，将软炭毡包裹在圆筒状的石墨筒上，再用钼丝系紧；炉底和炉顶则先垫几层软炭毡，再盖石墨盖板。由于石墨制品强度不好，往往设计得较厚，重量较大，吸收能量较多，且挤占空间；此外，石墨制品容易破损，使用寿命较短，更换频繁；大尺寸的石墨制品成形加工也较困难，难以满足生产的需求；在包裹软炭毡时，会产生大量碳尘，污染环境，刺激人的皮肤和渗入到人的呼吸系统，影响工人健康；此外，软炭毡在使用过程中容易损坏，包裹时操作麻烦，费时费力。专利申请号为200710017915.3，公开日为2007年10月31日的专利申请，公开了一种单晶硅拉制炉用炭/炭保温罩的制备方法，该方法采用炭纤维无纬布与薄炭纤维网胎交替环向缠绕，径向针刺制成低密度准三向保温罩预制体；通过糠酮树脂真空浸渍、固化和炭化致密保温罩预制体，反复致密2～4次，达到密度≥1.2g/cm3时，致密工艺结束，在通入氯气或氟利昂的条件下，进行高温纯化处理，机加工后即制备单晶拉制炉用炭/炭保温罩。其过程较为复杂，周期较长；要通入氯气和氟利昂对制品进行纯化处理，对环保带来一定的压力，在人们环保意识日益增强的今天，这也是人们所不希望的，产品保温性能欠佳，其导热系数为6W/mK-10W/mK(300K)(见实施例)。
专利申请号为200610136811.X，公开日为2007年07月11目的专利申请，公开了一种硅晶体生长炉用高纯固化炭毡制造方法，该方法选择金属杂质含量低的软的毡体作坯体材料，高温预处理使之成为石墨毡体；用石墨毡体制作坯体；对均匀渗入固化剂的坯体进行固化定型；炭化处理坯体；再对坯体进行化学气相预沉积；对零件的部分需切削加工的表面进行机械切削加工；再对坯体高温处理，去除金属杂质和挥发分；对出炉后的零件已加工面进行表面深层处理及零件的表面强化处理，提高坯体表面抗侵蚀能力。该方法在对坯体进行化学气相预沉积前，要先进行坯体材料高温预处理；然后再将经高温预处理的毡体制成坯体，继而还要对坯体进行固化定型及炭化处理，过程较为复杂，周期较长，且在处理过程中也可能将杂质带入坯体中。
发明内容：
本发明的目的是提供一种工艺简单、导热系数小的高温炉用固化碳纤维保温材料及其生产工艺。
本发明是采用如下技术方案实现其发明目的的，一种高温炉用固化碳纤维保温材料的生产工艺，它包括以下步骤：
(1)预制体制备：
①开松成网：选取6mm-70mm长的短碳纤维，经开松设备开松成蓬松的针状纤维，然后把开松好的碳纤维经气流成网和/或梳理成网，再利用铺网机铺成纤维网，预刺成网胎；
②叠层复合：把所得的网胎根据所需要求，通过针刺使之复合，制成板状或条状或圆筒状等预制体；
(2)增密：将步骤(1)所得的预制体经化学气相沉积增密，并经石墨化处理，制成保温材料坯体；
(3)热振纯化：将步骤(2)所得保温材料坯体放入高温炉中，在真空或保护气氛条件下进行热振纯化处理，制成固化碳纤维保温材料；
(4)机加工：将步骤(3)所得固化碳纤维保温材料机加工成所需形状和尺寸的制品。
本发明为使步骤(4)所得固化碳纤维保温材料制品不掉灰，并增加其抗腐蚀和抗冲刷的能力，进行步骤(5)表面处理，即将步骤(4)所得制品进行化学气相沉积处理，使制品的表面形成一层10mm-50mm厚的沉积碳，温度1100℃-1300℃，时间5小时-30小时。
本发明为去除机加工过程中可能带进的杂质，进行步骤(6)净化，即将步骤(5)所得制品在真空或保护气氛条件下进行净化处理，以去除机加工过程中可能带进的杂质，温度为1800℃-2300℃，保温时间为1h-3h。
本发明在步骤(1)开松成网中，所述网胎的面密度为30g/m2-130g/m2。
本发明在步骤(1)叠层复合中，针刺深度为6mm-25mm；针刺密度3次/cm2-10次/cm2；层密度为3层/cm-20层/cm。
本发明在步骤(1)叠层复合中，所述预制体的表观密度≤0.3g/cm3。
本发明在步骤(2)中，所述保温材料坯体的表观密度≤0.5g/cm3。
本发明在步骤(3)中，纯化温度为2300℃-2800℃，保温时间为0.5h/次-2h/次，循环次数2次-3次。
一种由上述生产工艺生产的高温炉用固化碳纤维保温材料，它为板状或条状或圆筒状，经预制体制备-增密-热振纯化-机加工步骤制成或经预制体制备-增密-热振纯化-机加工-表面处理-净化步骤制成。
由于采用上述技术方案，本发明较好的实现了发明目的，在预制体制备中无须粘接、浸渍、固化和炭化等过程，其工艺简单且节能环保，预制体内部碳纤维纵横交错，抱合力较强，不会脱层，结构稳定，导热系数≤0.8W/mK，保温性能优良；产品由高强度碳纤维和碳素基质构成，具有高比强度、耐高温、耐腐蚀、保温性能好等优良性能，兼具耐火、保温双重特性，且能承载一定的重荷，是替代高温炉用相关石墨制品及软炭毡的理想的升级产品。
具体实施方式：
下面结合实施例对本发明作进一步说明。
实施例1：
一种高温炉用固化碳纤维保温材料的生产工艺，它包括以下步骤：
(1)预制体制备：
①开松成网：选取6mm-70mm长的短碳纤维(本实施例为15mm-50mm)，经开松设备开松成蓬松的针状纤维，然后把开松好的碳纤维经气流成网和/或梳理成网(本实施例为气流成网和梳理成网)，再利用铺网机铺成纤维网，预刺成网胎；所述网胎的面密度为30g/m2-130g/m2(本实施例为90g/m2)。
②叠层复合：把所得的网胎根据所需要求，通过针刺使之复合，制成板状或条状或圆筒状等预制体(本实施例为圆筒状)；针刺深度为6mm-25mm(本实施例为15mm)；针刺密度3次/cm2-10次/cm2(本实施例为6次/cm2)；层密度为3层/cm-20层/cm(本实施例为7层/cm)；所述预制体的表观密度≤0.3g/cm3(本实施例为0.26g/cm3)。
(2)增密：将步骤(1)所得的预制体经化学气相沉积增密，并经石墨化处理，制成保温材料坯体；所述保温材料坯体的表观密度≤0.5g/cm3(本实施例为0.48g/cm3)。
(3)热振纯化：将步骤(2)所得保温材料坯体放入高温炉中，在真空或保护气氛条件下进行热振纯化处理，制成固化碳纤维保温材料；纯化温度为2300℃-2800℃(本实施例为2300℃)，保温时间为0.5h/次-2h/次(本实施例为1h)，循环次数2次-3次(本实施例为2次)。即炉膛抽真空后加热，至2000℃后充入氩气，继续升温至2300℃，保温1h后，停止加热，至炉温冷至1500℃，停止供氩气，然后再抽真空15分钟后，恢复供电加热，同时充氩气，当炉温再次升至2300℃，保温0.5h，即停止加热，炉内工件随炉冷却至350℃以下出炉，所得固化碳纤维保温材料灰分≤30ppm。
(4)机加工：将步骤(3)所得固化碳纤维保温材料机加工成所需形状和尺寸的制品。
一种由上述生产工艺生产的高温炉用固化碳纤维保温材料，它为板状或条状或圆筒状(本实施例为圆筒状)，经预制体制备-增密-热振纯化-机加工步骤制成，其导热系数≤0.8W/mK(本实施例为0.7W/mK)，用作高温炉的耐火保温筒。
本发明使用时，为减少以辐射为传热方式的高温炉的热损失，可在固化碳纤维保温材料的内壁或表面设有表面平整光滑，粗糙度好的柔性石墨板。为提高固化碳纤维保温材料制品的抗侵蚀和抗冲刷能力，也可在其内壁或表面设有碳纤维布。
实施例2：
本发明在步骤(1)叠层复合中，制成板状预制体，其表观密度为0.18g/cm3，增密后其表观密度为0.39g/cm3，
本发明为使所得固化碳纤维保温材料板材不掉灰，并增加其抗腐蚀和抗冲刷的能力，进行步骤(5)表面处理，即将步骤(4)所得制品进行化学气相沉积处理，使制品的表面形成一层10mm-50mm厚的沉积碳(本实施例为)，温度1100℃-1300℃(本实施例为1200℃)，时间5小时-30小时(本实施例为25小时)。为去除机加工过程中可能带进的杂质，进行步骤(6)净化，即将步骤(5)所得制品在真空或保护气氛条件下进行净化处理，温度为1800℃-2300℃(本实施例为2000℃)，保温时间为1h-3h(本实施例为1h)。
一种由上述生产工艺生产的高温炉用固化碳纤维保温材料，它为板状或条状或圆筒状(本实施例为板状)，经预制体制备-增密-热振纯化-机加工-表面处理-净化步骤制成，其导热系数为0.3W/mK用作高温炉的保温隔热板。余同实施例1。

Claims (10)

1.一种高温炉用固化碳纤维保温材料的生产工艺，其特征是包括以下步骤：
(1)预制体制备：
①开松成网：选取6mm-70mm长的短碳纤维，经开松设备开松成蓬松的针状纤维，然后把开松好的碳纤维经气流成网和/或梳理成网，再利用铺网机铺成纤维网，预刺成网胎；
②叠层复合：把所得的网胎根据所需要求，通过针刺使网胎复合，制成板状或条状或圆筒状预制体；
(2)增密：将步骤(1)所得的预制体经化学气相沉积增密，并经石墨化处理，制成保温材料坯体；
(3)热振纯化：将步骤(2)所得保温材料坯体放入高温炉中，在真空或保护气氛条件下进行热振纯化处理，制成固化碳纤维保温材料；
(4)机加工：将步骤(3)所得固化碳纤维保温材料机加工成所需形状和尺寸的制品。
2.根据权利要求1所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是进行步骤(5)表面处理，即将步骤(4)所得制品进行化学气相沉积处理，使制品的表面形成一层10mm-50mm厚的沉积碳，温度1100℃-1300℃，时间5小时-30小时。
3.根据权利要求2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是进行步骤(6)净化，即将步骤(5)所得制品在真空或保护气氛条件下进行净化处理，以去除机加工过程中可能带进的杂质，温度为1800℃-2300℃，保温时间为1h-3h。
4.根据权利要求1或2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是步骤(1)开松成网中，所述网胎的面密度为30g/m2-130g/m2。
5.根据权利要求1或2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是步骤(1)叠层复合中，针刺深度为6mm-25mm；针刺密度3次/cm2-10次/cm2；层密度为3层/cm-20层/cm。
6.根据权利要求1或2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是步骤(1)叠层复合中，所述预制体的表观密度≤0.3g/cm3。
7.根据权利要求1或2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是步骤(2)中，所述保温材料坯体的表观密度≤0.5g/cm3。
8.根据权利要求1或2所述的高温炉用固化碳纤维保温材料的生产工艺，其特征是步骤(3)中，纯化温度为2300℃-2800℃，保温时间为0.5h/次-2h/次，循环次数2次-3次。
9.一种如权利要求1所述生产工艺生产的高温炉用固化碳纤维保温材料，其特征是它为板状或条状或圆筒状，经预制体制备-增密-热振纯化-机加工制成。
10.一种如权利要求3所述生产工艺生产的高温炉用固化碳纤维保温材料，其特征是它为板状或条状或圆筒状，经预制体制备-增密-热振纯化-机加工-表面处理-净化制成。
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