CN112960983B - 一种碳化硅陶瓷复合制品的制备方法 - Google Patents
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Abstract
本发明属于耐火材料制备领域,尤其是涉及一种碳化硅陶瓷复合制品的制备方法。该方法是以高纯碳化硅颗粒、造粒碳化硅、碳化硅微粉为主要原料,添加少量硅粉,加入有机结合剂,充分混合均匀,采用半干法成,在保护气氛下、2200~2500℃烧结2~10h。该方法实现了半干法成型,与湿法成型相比,该方法成型周期短,效率高,坯体最大尺寸可以超过350mm,且产品微观结构均匀、各项性能优异,降低了生产成本,是重结晶碳化硅材料制备技术的一次重大突破。
Description
技术领域
本发明属于耐火材料制备技术领域,主要涉及一种碳化硅陶瓷复合制品的制备方法。
背景技术
碳化硅属于强共价键化合物,具有力学强度大、热导率高、膨胀系数小、耐磨性能好、抗化学侵蚀性强、抗热震性能优异等优点;碳化硅制品种类多,发展速度快;先后经历了硅酸盐结合碳化硅制品、氮化物结合碳化硅制品到性能更先进的自结合碳化硅;碳化硅制品普遍采用半干法成型,如机压成型、等静压成型等,成型效率高,适合大规模工业化应用。碳化硅制品广泛应用于有色、钢铁、石化、高温窑具等行业。
重结晶碳化硅是一种SiC含量大于98%的碳化硅制品,其各项性能是系列碳化硅耐火材料中最优异的。目前,重结晶碳化硅主要用于高温窑具行业,产品制备工艺单一,普遍采用注浆成型,该种成型方法工艺环节耗时长,坯体需要后续加工,人工成本高,原料使用率低,重结晶碳化硅生产工艺的局限性限制了自身的使用范围。
查阅相关专利发现,现有技术中碳化硅陶瓷复合制品大多采用注浆成型方式,或者其它方式,与本专利有显著区别。如,专利(CN101798223A,一种致密碳化硅陶瓷的制备方法)采用碳化硅、硅、碳原料,外加氮化硅、硼或者碳化硼、钒类中的一种,混合粉末直接置入坩埚中加热;该专利中加入部分添加剂、且粉末直接加热,未经过机压工艺过程;此外,还有部分专利是多孔材料制备方法,或者涂料的制备方法,而本专利针对致密材料,其制备方法与上述专利有显著区别。
专利(CN103570353A,一种重结晶碳化硅及制件的工艺方法)采用碳化硅粉、硅粉、碳粉为原料,机压成型、2500℃下超高温烧结而成。该专利中采用了碳化硅粉较细(40-120目碳化硅粉),且组分中包含碳粉,难以实现机压方式成型;另外碳粉是阻碍机压成型的有害组分,且在高温烧结过程中难以完全反应,少量碳残余会显著危害制品性能。
发明内容
为解决上述技术问题,本发明的目的是提出一种碳化硅陶瓷复合制品的制备方法。
本发明为完成上述目的采用如下技术方案:
一种碳化硅陶瓷复合制品的制备方法,碳化硅陶瓷复合制品的组成及重量比为:碳化硅颗粒50-70%wt,造粒碳化硅占比15-25%wt,碳化硅微粉15-25%wt;并外加硅粉2-10%wt,外加有机结合机2-10%wt,充分混合均匀,半干法成型得到合格坯体,120-200℃、20-60h烘干得到合格干坯体,在保护气氛下2200~2500℃保温2~10h至烧结完成得到所需碳化硅陶瓷复合制品。
所述的碳化硅颗粒由粒度为3-0.088mm的碳化硅颗粒和粒度为0.088-0mm的碳化硅颗粒组成。
所述的造粒碳化硅由3.5-0.5µm碳化硅经造粒工艺制备而得,其粒度0.1-0.03mm。
碳化硅微粉由中位径为3.5-0.5µm碳化硅组成。
所述硅粉的粒度为0.1-0mm,。
有机结合剂中碳含量在20-80%wt;所述的有机结合剂为热固树脂、热塑性树脂中的一种。
所述的半干法成型为机压成型、等静压成型或捣打成型。
所述保护气氛为氩气、氦气等惰性气体保护气氛或真空气氛。
本发明提出的一种碳化硅陶瓷复合制品的制备方法,将重结晶碳化硅中的微粉分成两部分,一部分进行造粒,改善了微粉在半干法混料及成型性能,另一部分直接加入,最终实现了半干法成型方式;同时引入少量硅粉,吸收了有机结合剂分解而成的碳,生成了少量碳化硅,用以防止残碳的存在。与重结晶碳化硅制品相比,本发明有3个显著优点:第一,新产品突破薄壁类二维材料的束缚,实现了大型块体三维材料的跨越,是一种全新的制备方法;第二,新产品生产效率高,生产成本大幅度降低,极大提高新产品的市场竞争力;第三,新产品采用半干法成型,易实现机械化智能化生产,且坯体不需要后续加工,符合环境管控要求,环保投资低。
附图说明
图1为本发明的工艺流程图。
具体实施方式
结合给出实施例对本发明加以说明,但是不构成对本发明的任何限制。
结合图1,所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:以碳化硅颗粒、造粒碳化硅、碳化硅微粉为主要原料,添加少量硅粉,加入有机结合剂,充分混合均匀,采用半干法成型(如,机压成型或等静压成型),在保护气氛下、2200~2500℃烧结2~10h。 该制备方法创新点在于通过优化组成设计改变了注浆成型工艺的束缚,实现了机压成型或等静压成型,丰富了碳化硅陶瓷复合制品的制备方法。
实施例1:
分别称取粒径大于0.088mm小于等于3mm的碳化硅颗粒3000g,粒径小于等于0.088mm的碳化硅颗粒2000g,中位径为3.5µm的碳化硅微粉2000g,中位径30µm的碳化硅造粒粉3000g,粒度小于等于0.1mm的硅粉1050g,放入高速混炼机中预混合均匀;加入碳含量30%酚醛树脂1500g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2450℃烧结3小时。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.13%。
实施例2:
分别称取粒径大于0.088mm小于等于3mm的碳化硅颗粒4000g,粒径小于等于0.088mm的碳化硅颗粒1000g,中位径为2.5µm的碳化硅微粉2000g,中位径30µm的碳化硅造粒粉3000g,粒度小于等于0.1mm的硅粉1050g,放入高速混炼机中预混合均匀;加入碳含量50%酚醛树脂1500g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2350℃烧结3h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.24%。
实施例3:
分别称取粒径大于0.88mm小于等于3mm的碳化硅颗粒4000g,粒径小于等于0.088mm的碳化硅颗粒2000g,中位径为3.5µm的碳化硅微粉1500g,中位径30µm的碳化硅造粒粉2500g,粒度小于等于0.1mm的硅粉840g,放入高速混炼机中预混合均匀;加入碳含量30%酚醛树脂1200g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2300℃烧结6h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.06%。
实施例4:
分别称取粒径大于0.088mm小于等于3mm的碳化硅颗粒4000g,粒径小于等于0.088mm的碳化硅颗粒2000g,中位径为2.5µm的碳化硅微粉2000g,中位径30µm的碳化硅造粒粉2000g,粒度小于等于0.1mm的硅粉1250g,放入高速混炼机中预混合均匀;加入碳含量45%酚醛树脂1200g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2350℃烧结4h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.19%。
实施例5:
分别称取粒径大于等于0.088mm小于等于3mm的碳化硅颗粒3000g,粒径小于等于0.088mm的碳化硅颗粒2000g,中位径为0.5µm的碳化硅微粉1000g,中位径30µm的碳化硅造粒粉3000g,粒度小于等于0.1mm的硅粉840g,放入高速混炼机中预混合均匀;加入碳含量30%酚醛树脂1200g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2300℃烧结3h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.13%。
实施例6:
分别称取粒径大于0.088mm小于等于3mm的碳化硅颗粒5000g,粒径小于等于0.088mm的碳化硅颗粒2000g,中位径为3.5µm的碳化硅微粉1000g,中位径30µm的碳化硅造粒粉2000g,粒度小于等于0.1mm的硅粉1200g,放入高速混炼机中预混合均匀;加入碳含量50%酚醛树脂1000g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2400℃烧结3h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.13%。
实施例7:
分别称取粒径大于0.088mm小于等于3mm的碳化硅颗粒4000g,粒径小于等于0.088mm的碳化硅颗粒3000g,中位径为0.5µm的碳化硅微粉1000g,中位径30µm的碳化硅造粒粉2000g,粒度小于等于0.1mm的硅粉1100g,放入高速混炼机中预混合均匀;加入碳含量50%酚醛树脂1000g,混合出均匀的泥料;在摩擦压砖机中压制成230×114×65mm块体;烘干;在超高温碳化硅烧结炉中2200℃烧结8h。即得到高纯碳化硅复合陶瓷制品,其碳化硅含量99.35%。
各个实施例所制备碳化硅陶瓷复合制品的性能表如下所示:
Claims (7)
1.一种碳化硅陶瓷复合制品的制备方法,其特征在于:碳化硅陶瓷复合制品的组成及重量比为:碳化硅颗粒50-70%wt,造粒碳化硅占比15-25%wt,碳化硅微粉15-25%wt;并外加硅粉2-10%wt,外加有机结合机2-10%wt,充分混合均匀,半干法成型得到合格坯体,120-200℃、20-60h烘干得到合格干坯体,在保护气氛下2200~2500℃保温2~10h至烧结完成得到所需碳化硅陶瓷复合制品。
2.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:所述的碳化硅颗粒由粒度为3-0.088mm的碳化硅颗粒和粒度为0.088-0mm的碳化硅颗粒组成。
3.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:所述的造粒碳化硅由3.5-0.5µm碳化硅经造粒工艺制备而得,其粒度0.1-0.03mm。
4.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:碳化硅微粉由中位径为3.5-0.5µm碳化硅组成。
5.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:所述硅粉的粒度为0.1-0mm。
6.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:有机结合剂中碳含量在20-80%wt;所述的有机结合剂为热固性树脂、热塑性树脂中的一种。
7.如权利要求1所述的一种碳化硅陶瓷复合制品的制备方法,其特征在于:所述的半干法成型为机压成型、等静压成型或捣打成型。
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FR2911869B1 (fr) * | 2007-01-29 | 2011-05-20 | Saint Gobain Ct Recherches | Procede de fabrication d'un corps poreux ceramique a base de sic |
CN102020480B (zh) * | 2010-12-14 | 2013-02-20 | 攀枝花市万腾耐火材料有限责任公司 | 用于电炉渣/铁口的浇注料及浇注电炉渣/铁口的方法 |
CN102503431B (zh) * | 2011-10-27 | 2013-07-03 | 中钢集团洛阳耐火材料研究院有限公司 | 一种碳化硅陶瓷制品及制备方法 |
CN103641500A (zh) * | 2013-12-04 | 2014-03-19 | 杜峰 | 耐高温碳化硅板材制作方法 |
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