CN107162612A - 一种碳化硅坩埚及其制备方法 - Google Patents
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Abstract
本发明提供了一种碳化硅坩埚及其制备方法,所述碳化硅坩埚由主料和辅料制成,所述主料由以下重量份的原料组成:石墨25~35份,碳化硅45~55份,粘土15~20份,金属硅3~5份;所述辅料由以下重量份的原料组成:木质素磺酸盐0.5~2.5份,稀土化合物0.7~1.8份,釉料2~5份。本发明的碳化硅坩埚具有较高的抗弯强度和耐热震性,使用寿命更长;生产工艺成本低,操作简单,易于实现。
Description
技术领域
本发明涉及耐火材料技术领域,尤其涉及一种高耐热震性的碳化硅坩埚及其制备方法。
背景技术
坩埚,作为化学仪器的重要组成部分,它是熔化和精炼金属液体以及固液加热、反应的容器,是保证化学反应顺利进行的基础。随着对坩埚的研究不断的深入,基于坩埚的使用周期较短,越来越多的人更倾向于追求质美价廉的坩埚制品,新颖优质的坩埚层出不穷。由于碳化硅化学性能稳定、导热系数高、热膨胀系数低,所以碳化硅坩埚也逐渐被提出并研制。
碳化硅坩埚主要用于锻造工艺及有色金属铸造的应用中,作为塑料、陶瓷、玻璃、水泥、橡胶和药品制造所需的耐高温耐腐蚀产品及贵金属的回收与精炼、石油化学工业领域所需的耐腐蚀容器。现有的石墨碳化硅特种坩埚的配方以及工艺生产的成品因受生产技术的限制以及配方等的限制,导致所生产的产品平均寿命为55天,寿命太短,而且使用及生产成本不断增高,产生的废弃物也居高不下。
中国专利文献上公开了一种“坩埚”,其公告号为CN103298983A,该发明的坩埚产品不包括有机材料,基本上没有无机含氧材料,具有改善的寿命,并且可以重新使用多次。但是,该发明的坩埚产品烧结成本高,热膨胀系数大,弹性小,耐热震性差,导致急冷急热条件下坩埚易碎裂。因此,研究新型的坩埚及其生产工艺是本领域技术人员亟待解决的技术问题。
发明内容
本发明为了克服现有坩埚易碎裂,抗弯强度差的问题,提供了一种耐热震性能好、不易破裂的碳化硅坩埚。
本发明还提供了一种操作简单的碳化硅坩埚的制备方法。
为了实现上述目的,本发明采用以下技术方案:
一种碳化硅坩埚,所述碳化硅坩埚由主料和辅料制成,所述主料由以下重量份的原料组成:石墨25~35份,碳化硅45~55份,粘土15~20份,金属硅3~5份;所述辅料由以下重量份的原料组成:木质素磺酸盐0.5~2.5份,稀土化合物0.7~1.8份,釉料2~5份。
本发明在碳化硅坩埚配方的辅料中加入木质素磺酸盐,木质素磺酸盐具有一定的粘度,可以进一步提高碳化硅坩埚的抗弯强度和耐热震性,延长使用寿命,此外,木质素磺酸盐成本低,可以起到节约成本的作用。稀土化合物的加入,使得在碳化硅坩埚在烧制的过程中在坩埚中掺入少来能稀土元素,一方面可以减少釉层破裂并使其具有光泽,确保碳化硅坩埚的颜色更柔和、纯正,色调新颖,光洁度好,另一方面其优异的延展性有利于增强的碳化硅坩埚的抗弯强度和耐热震性。主要原理如下:稀土元素有未充满的4f电子,可以吸收或发射从紫外、可见到红外光区不同波长的光,发射每种光区的范围小,加入少量稀土,可以确保碳化硅坩埚的颜色更柔和、纯正,具有优异的抗弯强度和耐热震性。
作为优选,所述稀土化合物为三氧化二铈、硝酸铕、氯化镧中的一种或几种,这几种稀土元素的性能较佳,在碳化硅坩埚中添加少量,即可起到抗弯强度和耐热震性的提升。
作为优选,所述木质素磺酸盐选自木质素磺酸钠、木质素磺酸镁、木质素磺酸钙和木质素磺酸铵中的一种或多种。
选取常见的木质素磺酸钠成本较低,有利于企业节约成本,增大企业效益。
作为优选,所述釉料由膨润土、耐火粘土、玻璃粉、长石粉、羧甲基纤维素钠和水组成,该组份一方面可以对碳化硅坩埚上色,另一方面添加的羧甲基纤维素钠,既可以作为稳定剂,又可以作为增稠剂,可以增加碳化硅坩埚的耐热震性。
一种碳化硅坩埚的制备方法,包括以下步骤:
(1)按照上述配比进行配料得到主料,于混料机中混合均匀后待用;
(2)按照上述配比称取木质素磺酸盐和稀土化合物,于混料机中18~20℃混合均匀,边搅拌边加入到主料中,得到混合均匀的物料;
(3)将步骤(2)得到的物料放入模具,压制成型,自然干燥2~3天,得到坩埚坯;
(4)按照上述配比配制釉料,对步骤(3)得到的坩埚坯进行上釉,自然晾干后于1250~1350℃条件下烧制,常压烧结12~24h,随炉冷却后,得到碳化硅坩埚。
本发明具有如下有益效果:
(1)碳化硅坩埚具有较高的抗弯强度和耐热震性,使用寿命更长;
(2)生产工艺成本低,操作简单,易于实现。
具体实施方式
下面通过具体实施例,对本发明的技术方案作进一步具体的说明。
在本发明中,若非特指,所有设备和原料均可从市场购得或是本行业常用的,下述实施例中的方法,如无特别说明,均为本领域常规方法。
实施例1
(1)分别称取石墨25g,碳化硅45g,粘土15g,金属硅3g进行配料得到主料,于混料机中混合均匀后待用;
(2)分别称取木质素磺酸钠0.5g,硝酸铕1.2g,氯化镧0.6g,于混料机中18℃混合均匀,边搅拌边加入到主料中,得到混合均匀的物料;
(3)将步骤(2)得到的物料放入模具,压制成型,自然干燥2天,得到坩埚坯;
(4)称取膨润土0.7g,耐火粘土0.2g、玻璃粉0.15g,长石粉0.05g,羧甲基纤维素钠0.1g和水0.8g,配制成2g釉料,对步骤(3)得到的坩埚坯进行上釉,自然晾干后于1250℃条件下烧制,常压烧结12h,随炉冷却后,得到碳化硅坩埚。
实施例2
(1)分别称取石墨35g,碳化硅55g,粘土20g,金属硅5g进行配料得到主料,于混料机中混合均匀后待用;
(2)分别称取木质素磺酸镁1.5g,木质素磺酸1g和三氧化二铈0.7g,于混料机中20℃混合均匀,边搅拌边加入到主料中,得到混合均匀的物料;
(3)将步骤(2)得到的物料放入模具,压制成型,自然干燥3天,得到坩埚坯;
(4)称取膨润土1.4g,耐火粘土0.4g、玻璃粉0.3g,长石粉0.1g,羧甲基纤维素钠0.2g和水2.6g,配制成5g釉料,对步骤(3)得到的坩埚坯进行上釉,自然晾干后于1350℃条件下烧制,常压烧结24h,随炉冷却后,得到碳化硅坩埚。
实施例3
(1)分别称取石墨30g,碳化硅50g,粘土18g,金属硅4g进行配料得到主料,于混料机中混合均匀后待用;
(2)分别称取木质素磺酸钙0.7g,木质素磺酸铵0.8g,三氧化二铈0.7g,氯化镧0.5g,于混料机中19℃混合均匀,边搅拌边加入到主料中,得到混合均匀的物料;
(3)将步骤(2)得到的物料放入模具,压制成型,自然干燥2天,得到坩埚坯;
(4)称取膨润土1.0g,耐火粘土0.45g、玻璃粉0.28g,长石粉0.08g,羧甲基纤维素钠0.15g和水0.54g,配制成2.5g釉料,对步骤(3)得到的坩埚坯进行上釉,自然晾干后于1300℃条件下烧制,常压烧结18h,随炉冷却后,得到碳化硅坩埚。
对比例
对比例与实施例1的不同之处在于,对比例的配方中中未加入稀土化合物,其余工艺与实施例1完全相同。
对实施例1-3和对比例制得的碳化硅坩埚进行性能检测,结果如表1所示:
表1.理化指标结果
实施例1 | 实施例2 | 实施例3 | 对比例 | |
孔隙率,% | 7 | 6.5 | 5.5 | 9 |
耐受温度,℃ | 1250 | 1200 | 1300 | 1100 |
重复次数,次 | 6 | 8 | 7 | 3 |
根据表1的结果可以看出,本发明提供的碳化硅坩埚添加稀土化合物后相对于传统的坩埚具有孔隙率较低,耐受温度高,可重复使用,具有良好的抗热震性能,可进出≥1200℃炉膛,坩埚不炸裂。
本发明的碳化硅坩埚具有较高的抗弯强度和耐热震性,使用寿命更长,生产工艺成本低,操作简单,易于实现。
Claims (5)
1.一种碳化硅坩埚,其特征在于,所述碳化硅坩埚由主料和辅料制成,所述主料由以下重量份的原料组成:石墨25~35份,碳化硅45~55份,粘土15~20份,金属硅3~5份;所述辅料由以下重量份的原料组成:木质素磺酸盐0.5~2.5份,稀土化合物0.7~1.8份,釉料2~5份。
2.根据权利要求1所述的一种碳化硅坩埚,其特征在于,所述稀土化合物为三氧化二铈、硝酸铕、氯化镧中的一种或几种。
3.根据权利要求1所述的一种碳化硅坩埚,其特征在于,所述木质素磺酸盐选自木质素磺酸钠、木质素磺酸镁、木质素磺酸钙和木质素磺酸铵中的一种或多种。
4.根据权利要求1所述的一种碳化硅坩埚,其特征在于,所述釉料由膨润土、耐火粘土、玻璃粉、长石粉、羧甲基纤维素钠和水组成。
5.一种如权利要求1-4任一所述的碳化硅坩埚的制备方法,其特征在于,包括以下步骤:
(1)按照上述配比进行配料得到主料,于混料机中混合均匀后待用;
(2)按照上述配比称取木质素磺酸盐和稀土化合物,于混料机中18~20℃混合均匀,边搅拌边加入到主料中,得到混合均匀的物料;
(3)将步骤(2)得到的物料放入模具,压制成型,自然干燥2~3天,得到坩埚坯;
(4)按照上述配比配制釉料,对步骤(3)得到的坩埚坯进行上釉,自然晾干后于1250~1350℃条件下烧制,常压烧结12~24h,随炉冷却后,得到碳化硅坩埚。
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