CN114751755A - 一种碳化硅素胚及其制备方法 - Google Patents
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Abstract
本发明涉及一种碳化硅素胚及其制备方法,所述制备方法具体包括如下步骤:首先将适量碳化硅粉、炭黑、石墨粉和助剂加水后混合搅拌,得到混合配料;然后将混合配料注入压机挤出成型得到挤出坯体;干燥后得到素坯。本发明所述方法最终得到的素坯的密度ρ为2.10~2.4g/cm3,含水率≤0.1%,且质地和颜色均匀,且无炭黑团聚现象。且通过本发明所述方法,借助素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e,可以精确得到预先设定值的素坯密度,在实际生产过程中具有重大意义,有利于促进企业的经济生产。
Description
技术领域
本发明属于碳化硅陶瓷素坯制备技术领域,具体涉及一种反应烧结碳化硅 挤出素胚及其制备方法。
背景技术
碳化硅陶瓷具有热稳定性好、比刚度大等优良性能,开始在越来越多的领 域发挥重要作用。在众多的制备方法中,挤出成型制备碳化硅陶瓷因其制备成 本低、生产效率高,已经成为行业内最通用的成型方法,尤其是涉及结构较为 简单的产品。而碳化硅挤出素胚密度是整个成型工艺中最重要的参数之一,素 胚中的碳含量更是决定了产品的最终性能,因此需要对其进行严格的控制。现 有技术中的碳化硅挤出素胚,往往存在密度过大或过小或质地不均匀等问题。
发明内容
本发明的目的在于提供一种操作方便、密度均一且适宜的碳化硅素胚的制 备方法。
本发明的一种碳化硅素胚的制备方法,具体包括如下步骤:
(1)原料的混合:将碳化硅粉、炭黑、石墨粉和助剂加水后混合搅拌,得 到混合配料,所述混合配料中包含质量分数为4%~8%的炭黑(w2),2%~6% 的石墨粉(w3),1%~10%的助剂,10%~15%水(b),余量为碳化硅粉(w1); 所述助剂为纤维素、羧甲基纤维素钠、羟丙基甲基纤维素、聚乙烯醇、聚乙烯 吡咯烷酮、多糖类、甘油中的一种或多种;
(2)挤出成型:将步骤(1)中得到的混合配料注入压机挤出成型,设置 压缩比为0.94-0.99,挤压力为3~12MPa,挤压频率为8~10圈,挤压温度为10~35℃,真空度为零下0.085MPa以下,最终得到挤出坯体;
(3)烘干:将步骤(2)中得到的挤出坯体干燥后得到素坯,设置升温速 率为3~10℃/h,保温温度为45~70℃,保温时间为5~15h,自然冷却。
进一步,本发明所述制备方法步骤(3)中的素坯的密度ρ=(ρ1*n1*w1+ ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;
其中ρ1为碳化硅粉的堆积密度;n1为碳化硅粉的级配比例;
ρ2为炭黑的堆积密度;n2为炭黑的级配比例;
ρ3为石墨粉的堆积密度;n3为石墨粉的级配比例;
a为助剂系数,1≤a≤10;c为成型参数;d为烘干参数;e为常数。
进一步,本发明所述制备方法步骤(1)中所述碳化硅粉为球形,直径为 3~200um,且碳化硅粉的堆积密度ρ1为1.4g/cm3~1.5g/cm3;所述n1为5~30。 球形颗粒状的碳化硅粉末能够使得挤压过程更加平滑稳定,更易生成质地均匀 的坯体;而片状或不规则的原料粉末在挤压力的作用下相对更易发生定向排列, 而使得成型坯体呈现出各向异性。且级配比例n1也需适宜,若n1过大,则会 出现素坯粘合不住,强度太小的问题,若n1过小,又会导致素坯密度降低,粗 糙度太高的问题。
进一步,本发明所述制备方法步骤(1)中炭黑的堆积密度ρ2为 1.80g/cm3~1.85g/cm3;所述炭黑的级配比例n2为1~10。
进一步,本发明所述制备方法步骤(1)中的石墨粉的堆积密度ρ3为1.08 g/cm3~1.80g/cm3;所述石墨粉的级配比例n3为1~4。炭黑与石墨粉的级配比例 同样需要大小适宜,若n2或n3过小,则炭黑或石墨粉会团聚,导致反应不均、 产品开裂;而反之n2或n3过大,则原料的表面能过小,需要很高的能量才能 促使其发生反应,同样影响产品的最终性能,且尤其影响其强度。
进一步,本发明所述制备方法中的成型参数c为0.99~1.01。成型参数c与 挤压频率和成型素坯的截面积有关。当挤压频率固定不变,且素坯的截面积越 小时,需要的挤出压力越大,则成型参数越大,此时挤出坯体的密度变大,反 之亦然。而当素坯的截面积不变,且挤压频率越大时,也需要的挤出压力越大, 成型参数越大,密度越大。
进一步,本发明所述制备方法中的烘干参数d为1~1.7。烘干参数则主要取 决于升温速率,升温速率越快,该参数越小,素坯的密度越大,反之亦然。一 般来说,保温温度越低,保温时间越长,效果越好。若素坯未完全烘干,含水 率过高,则会导致素坯强度不够,影响后续烧结过程,烧结时发生坯体开裂。
进一步,本发明所述制备方法中的常数e为0.02~5.80。
本发明所述的碳化硅素坯,由上述任一所述的制备方法制成,所述素坯的 密度ρ为2.10~2.4g/cm3,含水率≤0.1%。
与现有技术相比,本发明具有以下有益的技术效果:
本发明所述的碳化硅素胚的制备方法操作简单,通过控制制备过程中选用 特定性质的原料,及合适的原料配比,并设定合适的挤压成型参数和烘干参数, 最终制得的素坯密度ρ为2.10~2.4g/cm3,含水率≤0.1%,且质地和颜色均匀, 且无炭黑团聚现象。该密度范围的素坯在经过后续烧结、打磨喷砂清洗之后, 产品最终烧结后的密度可达3.08g/cm3~3.16g/cm3,相比行业内相同产品约提高 5%,强度达200MPa~330MPa,约提高17%。另一方面,通过本发明所述方法, 借助素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e,可以精 确得到预先设定值的素坯密度,在实际生产过程中具有重大意义,有利于促进 企业的经济生产。
附图说明
图1为本发明实施例1中所述的烧结后最终成品的微观形貌图;
图2为本发明实施例1中所述的烘干工艺参数图。
具体实施方式
下面结合具体的实施例对本发明做进一步的详细说明。
实施例1:一种碳化硅素胚的制备方法,具体包括如下步骤:
(1)原料的混合:将碳化硅粉、炭黑、石墨粉和助剂加水后混合搅拌,得 到混合配料,所述混合配料中包含质量分数6%的炭黑(w2),5%的石墨粉(w3), 1%的助剂,15%的水(b),余量为碳化硅粉(w1);
由图2可知,其中碳化硅粉为球形,直径为3~200um,且碳化硅粉的堆积 密度ρ1为1.4g/cm3,级配比例n1为5;所述炭黑的堆积密度ρ2为1.80g/cm3, 级配比例n2为2;所述石墨粉的堆积密度ρ3为1.08g/cm3,级配比例n3为1。
(2)挤出成型:将步骤(1)中得到的混合配料注入压机挤出成型,设置 压缩比为0.95,挤压力为3~12MPa,挤压频率为8~10圈,挤压温度为10~35℃, 真空度为零下0.085MPa以下,最终得到挤出坯体;
(3)烘干:将步骤(2)中得到的挤出坯体干燥后得到素坯,设置升温速 率为5℃/h,保温温度为45℃,保温时间为10h,自然冷却,如图2所示。
本实施例1中最终得到的素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ 3*n3*w3)*a*b*c*d*e;其中a为助剂系数,a=1;成型参数c为1.01;烘干参 数d为1.5;常数e为2.6。
代入上述公式可得,本实施例1中所述的素坯的密度ρ为2.10g/cm3,且测 得所述的素坯含水率为0.1%。本实施例1中最终制得的素坯颜色和质地均匀, 由图1可知,烧结后最终成品同样外观良好且质地均匀,产品烧结后的密度为 3.10g/cm3,强度为280MPa。
实施例2:本实施例2与实施例1的不同之处仅在于,所述步骤(1)中助 剂含量为10%,则本实施例2中最终得到的素坯的密度ρ=(ρ1*n1*w1+ρ 2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a为助剂系数,a=10;成型参数c为 1.01;烘干参数d为1.5;常数e为0.27。
代入上述公式可得,本实施例2中所述的素坯的密度ρ为2.2g/cm3,且测得 所述的素坯含水率同样为0.1%,颜色和质地均匀。产品烧结后密度为3.12g/cm3, 强度为295MPa。
实施例3:本实施例3与实施例1的不同之处仅在于,所述步骤(1)中助 剂含量为2%,则本实施例3中最终得到的素坯的密度ρ=(ρ1*n1*w1+ρ 2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a为助剂系数,a=2;成型参数c为1.01; 烘干参数d为1.5;常数e为1.4。
代入上述公式可得,本实施例3中所述的素坯的密度ρ为2.28g/cm3,含水 率为0.05%,同样颜色和质地均匀。产品烧结后密度为3.15g/cm3,强度为 305MPa。
实施例4:本实施例4与实施例3的不同之处仅在于,所述步骤(1)中水 的含量为12%,则本实施例4中最终得到的素坯的密度ρ=(ρ1*n1*w1+ρ 2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a为助剂系数,a=2;成型参数c为1.01; 烘干参数d为1.5;常数e为1.2。
代入上述公式可得,本实施例4中所述的素坯的密度ρ为2.35g/cm3,含水 率为0.03%,同样颜色和质地均匀。产品烧结后密度为3.15g/cm3,强度为315MPa。
实施例5:本实施例5与实施例4的不同之处仅在于,所述步骤(1)中碳 化硅粉的堆积密度ρ1为1.45g/cm3,级配比例n1为20。则本实施例4中最终得 到的素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a 为助剂系数,a=2;成型参数c为1.01;烘干参数d为1.5;常数e为0.3。
代入上述公式可得,本实施例5中所述的素坯的密度ρ为2.4g/cm3,含水率 为0.05%,同样颜色和质地均匀。产品烧结后密度为3.15g/cm3,强度为320MPa。
实施例6:本实施例6与实施例5的不同之处仅在于,所述步骤(3)中烘 干过程的升温速率为5℃/h,保温温度为45~50℃,保温时间为15h,自然冷却 后得到的素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其 中a为助剂系数,a=2;成型参数c为1.01;烘干参数d为1.6;常数e为0.28。
代入上述公式可得,本实施例6中所述的素坯的密度ρ为2.41g/cm3,含水 率为0.01%,颜色和质地均匀。产品烧结后密度为3.16g/cm3,强度为330MPa。
对比例1:本对比例1与实施例6的不同之处仅在于,所述步骤(1)中助 剂含量为0.5%,水的含量为8%。则最终得到的素坯的密度ρ=(ρ1*n1*w1+ ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a为助剂系数,a=0.5;成型参数c 为1.01;烘干参数d为1.6;常数e为1.2。
代入上述公式可得,本对比例1中所述的素坯的密度ρ为1.72g/cm3,含水 率为0.03%。产品烧结后有裂缝,强度低,仅为180MPa。
对比例2:本对比例2与实施例6的不同之处仅在于,所述步骤(1)中碳 化硅粉的堆积密度ρ1为1.35g/cm3,级配比例n1为35。则最终得到的素坯的密 度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其中a为助剂系数, a=2;成型参数c为1.01;烘干参数d为1.6;常数e为0.12。
代入上述公式可得,本对比例2中所述的素坯的密度ρ为1.62g/cm3,含水 率为0.08%。产品烧结后有裂缝,强度低,仅为160MPa。
对比例3:本对比例3与实施例6的不同之处仅在于,所述步骤(3)中烘 干过程的升温速率为15℃/h,保温温度为45~50℃,保温时间为15h,自然冷却 后得到的素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;其 中a为助剂系数,a=2;成型参数c为1.01;烘干参数d为0.5;常数e为0.6。
代入上述公式可得,本对比例3中所述的素坯的密度ρ为1.6g/cm3,含水率 为0.2%。烧结后的产品发生开裂,密度低,为2.8g/cm3,强度也低,仅为190MPa。
综上所述,想要得到本发明所述的碳化硅素坯,其素坯的密度ρ为 2.10~2.4g/cm3,含水率≤0.1%。需在制备过程中满足如下步骤:
所述混合配料中包含质量分数为4%~8%的炭黑(w2),2%~6%的石墨粉 (w3),1%~10%的助剂,10%~15%水(b),余量为碳化硅粉(w1);挤出成 型过程中设置压缩比为0.94-0.99,挤压力为3~12MPa,挤压频率为8~10圈,挤 压温度为10~35℃,真空度为零下0.085MPa以下,最终得到挤出坯体;烘干过 程中设置升温速率为3~10℃/h,保温温度为45~70℃,保温时间为5~15h,然后 自然冷却。且素坯密度ρ的影响因素中,碳化硅粉的堆积密度ρ1为1.4g/cm3~1.5 g/cm3;级配密度n1为5~30;炭黑的堆积密度ρ2为1.80g/cm3~1.85g/cm3;级配 比例n2为1~10;墨粉的堆积密度ρ3为1.08g/cm3~1.80g/cm3,级配比例n3为 1~4;a为助剂系数,1≤a≤10;b混合后原料的含水量,为10%~15%;成型参 数c为0.99~1.01;烘干参数d为1~1.7;常数e为0.02~5.80。本发明所述素坯 在经过后续烧结、打磨喷砂清洗之后,产品最终烧结后的密度可达 3.08g/cm3~3.16g/cm3,强度达200MPa~330MPa,性能良好。
Claims (9)
1.一种碳化硅素胚的制备方法,其特征在于,具体包括如下步骤:
(1)原料的混合:将碳化硅粉、炭黑、石墨粉和助剂加水后混合搅拌,得到混合配料,所述混合配料中包含质量分数为4%~10%的炭黑(w2),2%~6%的石墨粉(w3),1%~10%的助剂,10%~15%水(b),余量为碳化硅粉(w1);
(2)挤出成型:将步骤(1)中得到的混合配料注入压机挤出成型,设置压缩比为0.94~0.99,挤压力为3~12MPa,挤压频率为8~10圈,挤压温度为10~35℃,真空度为零下0.085MPa以下,最终得到挤出坯体;
(3)烘干:将步骤(2)中得到的挤出坯体干燥后得到素坯,设置升温速率为3~10℃/h,保温温度为45~70℃,保温时间为5~15h,自然冷却。
2.根据权利要求1所述的碳化硅素胚的制备方法,其特征在于,所述步骤(3)中的素坯的密度ρ=(ρ1*n1*w1+ρ2*n2*w2+ρ3*n3*w3)*a*b*c*d*e;
其中ρ1为碳化硅粉的堆积密度;n1为碳化硅粉的级配比例;
ρ2为炭黑的堆积密度;n2为炭黑的级配比例;
ρ3为石墨粉的堆积密度;n3为石墨粉的级配比例;
a为助剂系数,1≤a≤10;c为成型参数;d为烘干参数;e为常数。
3.根据权利要求2所述的碳化硅素胚的制备方法,其特征在于,所述步骤(1)中所述碳化硅粉为球形,直径为3~200um,且碳化硅粉的堆积密度ρ1为1.4g/cm3~1.5g/cm3;所述n1为5~30。
4.根据权利要求2所述的碳化硅素胚的制备方法,其特征在于,所述步骤(1)中炭黑的堆积密度ρ2为1.80g/cm3~1.85g/cm3;所述炭黑的级配比例n2为1~10。
5.根据权利要求2所述的碳化硅素坯的制备方法,其特征在于,所述步骤(1)中的石墨粉的堆积密度ρ3为1.08g/cm3~1.80g/cm3;所述石墨粉的级配比例n3为1~4。
6.根据权利要求2所述的碳化硅素坯的制备方法,其特征在于,所述成型参数c为0.99~1.01。
7.根据权利要求2所述的碳化硅素坯的制备方法,其特征在于,所述烘干参数d为1~1.7。
8.根据权利要求2所述的碳化硅素坯的制备方法,其特征在于,所述常数e为0.02~5.80。
9.一种碳化硅素坯,其特征在于,所述素坯为权利要求1-8任一所述的制备方法制成,所述素坯的密度ρ为2.10~2.4g/cm3,含水率≤0.1%。
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