CN111138207A - 一种直拉单晶硅炉用石墨热场材料制备方法 - Google Patents
一种直拉单晶硅炉用石墨热场材料制备方法 Download PDFInfo
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Abstract
本发明涉及石墨热场技术领域,更具体而言,涉及一种直拉单晶硅炉用石墨热场材料制备方法,骨料为针状石油焦;粉料为石墨烯、沥青焦、炭黑、碳纤维;粘结剂为改质中温煤沥青;浸渍剂为浸渍沥青,中原料选择合理,制备工艺科学;所制备的直拉单晶硅炉用石墨热场材料结构均匀细腻,体积密度高;石墨理化理指标优良;石墨热场材料的体积密度≥2.0g/cm3,电阻率≤6.0μΩm,抗折强度≥32Mpa,抗压强度≥65Mpa,气孔率≤10%,灰分≤0.2%,热膨胀系数≤2*10‑6/℃。
Description
技术领域
本发明涉及石墨热场技术领域,更具体而言,涉及一种直拉单晶硅炉用石墨热场材料制备方法。
背景技术
直拉单晶炉的热系统,也就是所谓的热场,是指为了熔化硅料,并使单晶生长保持在一定温度下进行的整个系统。 石墨热场简单的说就是用来拉单晶硅的整套石墨加热系统。常见的是18寸、22寸和24寸的石墨热场。
热场一般包括(石墨材料)压环、保温盖、上中下保温罩、石墨坩埚(三瓣埚)、坩埚托杆、坩埚托盘、电极、加热器、导流筒、石墨螺栓,且为了防止漏硅,炉底、金属电极、托杆、都设置了保护板、保护套。
石墨在直拉单晶硅炉以高纯石墨、碳毡和碳薄三种形式在应用,石墨器件在炉內的化学反应是:C+SiO2→SiO+CO,SiO+2C→SiC+CO。
以上化学反应对石墨坩埚、加热器和保温筒产生以下影响:
一、石墨坩埚
1、石墨坩埚的內侧面发生上面的化学反应,在分瓣面附近R(圆角)部分发生消耗,其厚度变薄,由于Sic的生成,內侧面发生体积膨胀,引起坩埚的变形,分瓣面上部开裂等不良现象。2、坩埚的外侧面由于Si蒸汽或SiO气体而发生Si蒸汽的凝结,并出现SiC现象,但是SiC的生成的厚度比內侧面薄。3、外侧面的Si凝结多的时候,在R部形成滴状残留。
二、加热器1、发热部分的上半部正对着坩埚,温度较高,由于与SiO气体的反应引起消耗,厚度及宽度变小。2、发热部分的下半部温度较低,有Si蒸结及生成SiC现象。
三、保温筒1、內侧面与SiO气体反应,生成SiC,使体积膨胀,可能发生保温筒变形、裂缝等现象; 2、温度低的情况下,內侧面的下部分有Si蒸结现象。
在直拉单晶硅热场中使用的是各向同性石墨,其特点是:
1、石墨粒子各向均匀排列,特性与尺寸、形状、取料方向无关;2、强度高,不易破裂; 3、粒子直径小,密度高;4、传热、受热、放热均匀,温度分布均匀;5、与石英坩埚及上叙各种气体的反应小,消耗小,寿命长; 6、承压能力强,渐少各种可能的歪斜和破裂。
石墨材料不仅在民用上大有作为,在国防尖端上占有重要地位,属新型材料,令人瞩目。它是制造单晶炉、金属连铸石墨结晶器、电火花加工用石墨电极等不可替代的材料,更是制造火箭喷嘴、石墨反应堆的减速材料和反射材料的绝好材料。
发明内容
为了克服现有技术中所存在的不足,本发明提供一种直拉单晶硅炉用石墨热场材料制备方法,生产出各理化性能优质的新型细颗粒、高密度、高纯度石墨热场材料。
为了解决上述技术问题,本发明所采用的技术方案为:
一种直拉单晶硅炉用石墨热场材料制备方法,包括以下步骤:
S1、破碎、筛分、配料是将骨料、粉料按上述粒径进行筛分并配料;
S2、混捏:将经分级的配料加入混捏锅中进行搅拌,混捏分为干混和湿混,所述干混是将骨料和粉料加入混捏锅中进行搅拌,混捏锅为双铰刀式,混捏锅温度为220-250℃,骨料粉料干混温度为150-180℃,干混时间为45-50分钟;湿混粘结剂温度为140-180℃,湿混时间为40-45分钟;
S3、等静压成型:将混合均匀的粉料装入橡胶模具中,封口,冷等静压成型,成型后的生坯体积密度为1.8-2.2g/cm3;首先抽真空至10KPa~30KPa,再移至等静压机中压制成型,压型压力为100MPa~150MPa,先以10~12MPa/min的升压速率上升至所设定成型压力,稳压5~10min,再以8~12MPa/min的泄压速率泄压至80~90MPa,稳压5~10min;再以8~12MPa/min的泄压速率泄压至40~50MPa,稳压2~5min;最后以8~12MPa/min的泄压速率泄压至室压;然后置于水中冷却至常温;成型后的生坯的体积密度达到1.80-2.0g/cm3;
S4、一次焙烧:将成型生坯置入环式焙烧炉中,使用焦粉、石英砂、河砂等填充炉内,在隔绝空气的情况下,按升温曲线逐步加热,在150-350℃时,升温速率为3.0-4.0℃/h,保持时间55h;在350-450℃时,升温速率为1.5-1.8℃/h,保持时间35h;在450-550℃时,升温速率为1.2-1.4℃/h,保持时间85h;在550-650℃时,升温速率为1.8-2.0℃/h,保持时间55h;在650-750℃时,升温速率为3.5-4.0℃/h,保持时间24h;在750-850℃时,升温速率为4.0-5.0℃/h,保持时间24h;在850-1150℃时,升温速率为6.5-8.5℃/h,保持时间30h;在1150-1250℃时,升温速率为8.0-8.5℃/h,保持时间24h;在1250℃时保持22h,然后自然冷却至室温出炉;
S5、浸渍:将焙烧产品置入浸渍罐中,在一定工艺条件下,使浸渍剂浸渍沥青浸入焙烧产品孔隙中;首先将焙烧产品预热到350-450℃,保持时间8h,入浸渍罐,抽真空,加压2.5h,然后将浸渍剂注入浸渍罐中,保压2h;浸渍增重率15-17%;
S6、隧道窑二次焙烧:将浸渍后的产品经过隧道窑炉进行快速烧结沥青的过程,最高温度为700℃,时间144h;
S7、石墨化:将二次焙烧后的产品放入艾奇逊石墨化炉中,在隔绝空气的条件下,通过电流将焙烧品加热到2800-3200℃,具体为以250℃/h的升温速率,从室温升温到1350℃,然后以25℃/h的升温速度从1350℃升温到2200℃,温度达到2200℃以后自由升温至3200℃,使二维结构炭制品转换为三维石墨网格结构,送电总时间168h;
S8、机加工石墨化的制品经过机加工即得成品。
进一步地,所述骨料为针状石油焦;粉料为石墨烯、沥青焦、炭黑、碳纤维;粘结剂为改质中温煤沥青;浸渍剂为浸渍沥青。
进一步地,所述骨料针状石油焦的真密度≥2.13g/cm3,灰分≤0.20%,挥发分≤0.25%,硫含量≤0.30%;
所述粉料石墨烯的拉伸模量≤1.01TPa,极限强度≤116Gpa,粒径为0.02-0.06μm;
所述粉料沥青焦的粒度为0.05-0.10μm、真密度≥2.13/cm3,灰分≤0.25%、含硫量≤0.3%、挥发份≤0.5%;
所述粉料炭黑的纯度99%,粒径为0.04-0.08μm;
所述粉料碳纤维的粒度为0.03-0.07μm、抗拉强度7.0Gpa、密度2.10g/cm3、电阻率≤35μΩcm;
所述粘结剂改质中温煤沥青的软化点为83-86℃,结焦值为≥52%,灰分≤0.30%;
所述浸渍剂浸渍沥青的软化点为83-88℃,结焦值为≥52%,喹啉不溶物≤0.30%。
进一步地,所述粉料粉料石墨烯、沥青焦、炭黑、碳纤维的重量比为20:30:15:35。
进一步地,所述骨料、粉料的重量比为70:30-72:28。
进一步地,按重量百分含量计,所述针状石油焦破碎的粒径范围与含量为:
粒径1μm-0.5μm 20wt%;
粒径0.5μm-0.3μm 25wt%;
粒径0.3μm-0.1μm 20wt%;
粒径0-0.1μm 45wt%。
进一步地,所述浸渍剂注入浸渍罐前经超声处理。
进一步地,所述超声处理能量为38J,超声处理时间为30min。
与现有技术相比,本发明所具有的有益效果为:
本发明提供了一种直拉单晶硅炉用石墨热场材料制备方法,骨料为针状石油焦;粉料为石墨烯、沥青焦、炭黑、碳纤维;粘结剂为改质中温煤沥青;浸渍剂为浸渍沥青,原料选择合理,制备工艺科学;所制备的直拉单晶硅炉用石墨热场材料结构均匀细腻,体积密度高;石墨理化理指标优良;石墨热场材料的体积密度≥2.0g/cm3,电阻率≤6.0μΩm,抗折强度≥32Mpa,抗压强度≥65Mpa,气孔率≤10%,灰分≤0.2%,热膨胀系数≤2*10-6/℃。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
一种直拉单晶硅炉用石墨热场材料制备方法,包括以下步骤:
S1、破碎、筛分、配料是将骨料、粉料按上述粒径进行筛分并配料;
S2、混捏:将经分级的配料加入混捏锅中进行搅拌,混捏分为干混和湿混,所述干混是将骨料和粉料加入混捏锅中进行搅拌,混捏锅为双铰刀式,混捏锅温度为220-250℃,骨料粉料干混温度为150-180℃,干混时间为45-50分钟;湿混粘结剂温度为140-180℃,湿混时间为40-45分钟;
S3、等静压成型:将混合均匀的粉料装入橡胶模具中,封口,冷等静压成型,成型后的生坯体积密度为1.8-2.2g/cm3;首先抽真空至10KPa~30KPa,再移至等静压机中压制成型,压型压力为100MPa~150MPa,先以10~12MPa/min的升压速率上升至所设定成型压力,稳压5~10min,再以8~12MPa/min的泄压速率泄压至80~90MPa,稳压5~10min;再以8~12MPa/min的泄压速率泄压至40~50MPa,稳压2~5min;最后以8~12MPa/min的泄压速率泄压至室压;然后置于水中冷却至常温;成型后的生坯的体积密度达到1.80-2.0g/cm3;
S4、一次焙烧:将成型生坯置入环式焙烧炉中,使用焦粉、石英砂、河砂等填充炉内,在隔绝空气的情况下,按升温曲线逐步加热,在150-350℃时,升温速率为3.0-4.0℃/h,保持时间55h;在350-450℃时,升温速率为1.5-1.8℃/h,保持时间35h;在450-550℃时,升温速率为1.2-1.4℃/h,保持时间85h;在550-650℃时,升温速率为1.8-2.0℃/h,保持时间55h;在650-750℃时,升温速率为3.5-4.0℃/h,保持时间24h;在750-850℃时,升温速率为4.0-5.0℃/h,保持时间24h;在850-1150℃时,升温速率为6.5-8.5℃/h,保持时间30h;在1150-1250℃时,升温速率为8.0-8.5℃/h,保持时间24h;在1250℃时保持22h,然后自然冷却至室温出炉;
S5、浸渍:将焙烧产品置入浸渍罐中,在一定工艺条件下,使浸渍剂浸渍沥青浸入焙烧产品孔隙中;首先将焙烧产品预热到350-450℃,保持时间8h,入浸渍罐,抽真空,加压2.5h,然后将浸渍剂注入浸渍罐中,保压2h;浸渍增重率15-17%;
S6、隧道窑二次焙烧:将浸渍后的产品经过隧道窑炉进行快速烧结沥青的过程,最高温度为700℃,时间144h;
S7、石墨化:将二次焙烧后的产品放入艾奇逊石墨化炉中,在隔绝空气的条件下,通过电流将焙烧品加热到2800-3200℃,具体为以250℃/h的升温速率,从室温升温到1350℃,然后以25℃/h的升温速度从1350℃升温到2200℃,温度达到2200℃以后自由升温至3200℃,使二维结构炭制品转换为三维石墨网格结构,送电总时间168h;
S8、机加工石墨化的制品经过机加工即得成品。包括:压环、保温盖、上中下保温罩、石墨坩埚(三瓣埚)、坩埚托杆、坩埚托盘、电极、加热器、导流筒、石墨螺栓,且为了防止漏硅,炉底、金属电极、托杆、都设置了保护板、保护套。
在本实施例中,所述骨料为针状石油焦;粉料为石墨烯、沥青焦、炭黑、碳纤维;粘结剂为改质中温煤沥青;浸渍剂为浸渍沥青。
在本实施例中,所述骨料针状石油焦的真密度≥2.13g/cm3,灰分≤0.20%,挥发分≤0.25%,硫含量≤0.30%;
所述粉料石墨烯的拉伸模量≤1.01TPa,极限强度≤116Gpa,粒径为0.02-0.06μm;
所述粉料沥青焦的粒度为0.05-0.10μm、真密度≥2.13/cm3,灰分≤0.25%、含硫量≤0.3%、挥发份≤0.5%;
所述粉料炭黑的纯度99%,粒径为0.04-0.08μm;
所述粉料碳纤维的粒度为0.03-0.07μm、抗拉强度7.0Gpa、密度2.10g/cm3、电阻率≤35μΩcm;
所述粘结剂改质中温煤沥青的软化点为83-86℃,结焦值为≥52%,灰分≤0.30%;
所述浸渍剂浸渍沥青的软化点为83-88℃,结焦值为≥52%,喹啉不溶物≤0.30%。
在本实施例中,所述粉料粉料石墨烯、沥青焦、炭黑、碳纤维的重量比为20:30:15:35。
在本实施例中,所述骨料、粉料的重量比为70:30-72:28。
在本实施例中,按重量百分含量计,所述针状石油焦破碎的粒径范围与含量为:
粒径1μm-0.5μm 20wt%;
粒径0.5μm-0.3μm 25wt%;
粒径0.3μm-0.1μm 20wt%;
粒径0-0.1μm 45wt%。
在本实施例中,所述浸渍剂注入浸渍罐前经超声处理。减少沥青在浸渍过程中重油难溶组分的聚集,同时降低沥青粘度。
在本实施例中,所述超声处理能量为38J,超声处理时间为30min。
上面仅对本发明的较佳实施例作了详细说明,但是本发明并不限于上述实施例,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化,各种变化均应包含在本发明的保护范围之内。
Claims (8)
1.一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于,包括以下步骤:
S1、破碎、筛分、配料是将骨料、粉料进行筛分并配料;
S2、混捏:将经分级的配料加入混捏锅中进行搅拌,混捏分为干混和湿混,所述干混是将骨料和粉料加入混捏锅中进行搅拌,混捏锅为双铰刀式,混捏锅温度为220-250℃,骨料粉料干混温度为150-180℃,干混时间为45-50分钟;湿混粘结剂温度为140-180℃,湿混时间为40-45分钟;
S3、等静压成型:将混合均匀的粉料装入橡胶模具中,封口,冷等静压成型,成型后的生坯体积密度为1.8-2.2g/cm3;首先抽真空至10KPa~30KPa,再移至等静压机中压制成型,压型压力为100MPa~150MPa,先以10~12MPa/min的升压速率上升至所设定成型压力,稳压5~10min,再以8~12MPa/min的泄压速率泄压至80~90MPa,稳压5~10min;再以8~12MPa/min的泄压速率泄压至40~50MPa,稳压2~5min;最后以8~12MPa/min的泄压速率泄压至室压;然后置于水中冷却至常温;成型后的生坯的体积密度达到1.80-2.0g/cm3;
S4、一次焙烧:将成型生坯置入环式焙烧炉中,使用焦粉、石英砂、河砂等填充炉内,在隔绝空气的情况下,按升温曲线逐步加热,在150-350℃时,升温速率为3.0-4.0℃/h,保持时间55h;在350-450℃时,升温速率为1.5-1.8℃/h,保持时间35h;在450-550℃时,升温速率为1.2-1.4℃/h,保持时间85h;在550-650℃时,升温速率为1.8-2.0℃/h,保持时间55h;在650-750℃时,升温速率为3.5-4.0℃/h,保持时间24h;在750-850℃时,升温速率为4.0-5.0℃/h,保持时间24h;在850-1150℃时,升温速率为6.5-8.5℃/h,保持时间30h;在1150-1250℃时,升温速率为8.0-8.5℃/h,保持时间24h;在1250℃时保持22h,然后自然冷却至室温出炉;
S5、浸渍:将焙烧产品置入浸渍罐中,在一定工艺条件下,使浸渍剂浸渍沥青浸入焙烧产品孔隙中;首先将焙烧产品预热到350-450℃,保持时间8h,入浸渍罐,抽真空,加压2.5h,然后将浸渍剂注入浸渍罐中,保压2h;浸渍增重率15-17%;
S6、隧道窑二次焙烧:将浸渍后的产品经过隧道窑炉进行快速烧结沥青的过程,最高温度为700℃,时间144h;
S7、石墨化:将二次焙烧后的产品放入艾奇逊石墨化炉中,在隔绝空气的条件下,通过电流将焙烧品加热到2800-3200℃,具体为以250℃/h的升温速率,从室温升温到1350℃,然后以25℃/h的升温速度从1350℃升温到2200℃,温度达到2200℃以后自由升温至3200℃,使二维结构炭制品转换为三维石墨网格结构,送电总时间168h;
S8、机加工石墨化的制品经过机加工即得成品。
2.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述骨料为针状石油焦;粉料为石墨烯、沥青焦、炭黑、碳纤维;粘结剂为改质中温煤沥青;浸渍剂为浸渍沥青。
3.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述骨料针状石油焦的真密度≥2.13g/cm3,灰分≤0.20%,挥发分≤0.25%,硫含量≤0.30%;
所述粉料石墨烯的拉伸模量≤1.01TPa,极限强度≤116Gpa,粒径为0.02-0.06μm;
所述粉料沥青焦的粒度为0.05-0.10μm、真密度≥2.13/cm3,灰分≤0.25%、含硫量≤0.3%、挥发份≤0.5%;
所述粉料炭黑的纯度99%,粒径为0.04-0.08μm;
所述粉料碳纤维的粒度为0.03-0.07μm、抗拉强度7.0Gpa、密度2.10g/cm3、电阻率≤35μΩcm;
所述粘结剂改质中温煤沥青的软化点为83-86℃,结焦值为≥52%,灰分≤0.30%;
所述浸渍剂浸渍沥青的软化点为83-88℃,结焦值为≥52%,喹啉不溶物≤0.30%。
4.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述粉料粉料石墨烯、沥青焦、炭黑、碳纤维的重量比为20:30:15:35。
5.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述骨料、粉料的重量比为70:30-72:28。
6.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:按重量百分含量计,所述针状石油焦破碎的粒径范围与含量为:
粒径1μm-0.5μm 20wt%;
粒径0.5μm-0.3μm 25wt%;
粒径0.3μm-0.1μm 20wt%;
粒径0-0.1μm 45wt%。
7.根据权利要求1所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述浸渍剂注入浸渍罐前经超声处理。
8.根据权利要求7所述的一种直拉单晶硅炉用石墨热场材料制备方法,其特征在于:所述超声处理能量为38J,超声处理时间为30min。
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CN114014662A (zh) * | 2021-09-28 | 2022-02-08 | 大同新成新材料股份有限公司 | 一种硒-石墨烯复合型等静压石墨材料及其制备方法 |
WO2023072613A1 (de) * | 2021-11-01 | 2023-05-04 | Nippon Kornmeyer Carbon Group Gmbh | Verfahren zur herstellung von carbonisierten oder graphitierten 3d-gegenständen |
CN115259870A (zh) * | 2022-07-29 | 2022-11-01 | 宝丰县洁石碳素材料有限公司 | 一种单晶热场用石墨的制备工艺 |
WO2024032910A1 (de) * | 2022-08-10 | 2024-02-15 | Nippon Kornmeyer Carbon Group Gmbh | Verfahren zur herstellung von graphit |
CN116789453A (zh) * | 2023-04-19 | 2023-09-22 | 湖北东南佳特碳新材料有限公司 | 一种石墨坩埚及其制备方法和应用 |
CN116789453B (zh) * | 2023-04-19 | 2024-03-19 | 湖北东南佳特碳新材料有限公司 | 一种石墨坩埚及其制备方法和应用 |
CN116903373A (zh) * | 2023-07-28 | 2023-10-20 | 鄯善隆盛碳素制造有限公司 | 石墨化炉头护板加工工艺 |
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