CN112939604A - 一种高导热碳化硅材料及其制备方法 - Google Patents
一种高导热碳化硅材料及其制备方法 Download PDFInfo
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Abstract
本申请涉及机械密封件材料领域,具体公开了一种高导热碳化硅材料及其制备方法。高导热碳化硅材料由以下重量份数的原料组成:碳化硅65‑75份,金刚石3‑10份,石墨粉18‑22份,粘结剂1‑5份,助烧剂2‑10份、硼粉1‑3份和硅片5‑15份;其制备方法为:S1、根据配方比例称取各原料,加水混合均匀,得到料浆;S2、将S1中的料浆经喷雾干燥造粒,得到颗粒;S3、将S2中的颗粒压制成型,得到素坯;S4、将S3中的素坯烘焙成型,然后进行加工;S5、真空烧结,经自然冷却后得到高导热碳化硅材料。本申请的高导热碳化硅材料可用于制备机械密封环,其具有良好的热传导性能。
Description
技术领域
本申请涉及机械密封件材料领域,更具体地说,它涉及一种高导热碳化硅材料及其制备方法。
背景技术
碳化硅是一种理想的密封材料,具有优良的耐化学腐蚀性能,较高的机械强度,良好的耐磨性能、耐高温性能和自润滑性能,碳化硅的摩擦系数小且具有优异的热传导性。碳化硅作为高温结构材料,已广泛地应用于石油、化工、机械、军工、船舶、航天和汽车等领域,并可广泛地用作机械密封的摩擦副材料。
但是由于碳化硅的共价键很强,导致其高温扩散系数非常低,在2100℃的高温下,C和Si的自扩散系数分别为1.5×10-10cm2/s和2.5×10-13cm2/s,难以烧结成致密材料。
碳化硅材料用于制备机械密封环时,由于机械密封件工作时处于高速旋转容易摩擦产生热量,热量若不及时散发出去,机械密封件容易发生损坏,故机械密封件对热传导性能的要求很高,需要进一步提高碳化硅材料的导热系数。
发明内容
为了提高碳化硅的导热系数,本申请提供一种高导热碳化硅材料及其制备方法。
第一方面,本申请提供一种高导热碳化硅材料,采用如下的技术方案:
一种高导热碳化硅材料,由以下重量份数的原料组成:碳化硅65-75份,金刚石3-10份,石墨粉18-22份,粘结剂1-5份,助烧剂2-10份、硼粉1-3份和硅片5-15份。
通过采用上述技术方案,金刚石的添加提高了高导热碳化硅材料的导热系数,机械密封环在工作时会因摩擦而产生大量热量,由于提高了导热碳化硅材料的导热系数,机械密封环所产生的热量能够得到有效的散发,从而使得该机械密封环具有良好的散热性能。同时金刚石的添加能够增加导热碳化硅材料的硬度,从而提高由该材料制备的机械密封环的耐磨性能以及机械强度,延长了机械密封环的使用寿命。
碳化硅与石墨粉在反应过程中能够经过加热与液态Si反应生成β-SiC,从而提高产品强度,起到增加断裂韧性的效果。同时,由于原料中添加有石墨粉,当密封件处于高速旋转时会发生摩擦磨损,在摩擦磨损过程中,石墨不断向表面挤出,逐渐伸展并被压平成连续完成的固体润滑膜,起到自润滑作用,从而减小摩擦力。
优选的,所述粘结剂为聚乙烯醇、乙基羟甲基纤维素和明胶中的至少一种。
通过采用上述技术方案,聚乙烯醇、乙基羟甲基纤维素和明胶均属于水基粘接剂,由于碳化硅属于极性固体粉体,具有亲水性,且水基粘接剂与碳化硅粉末不发生化学反应,具有良好的流变特性、注射成型和保形性好等特点。
优选的,所述助烧剂为水溶性酚醛树脂和丙烯酸中的其中一种。
通过采用上述技术方案,由于SiC是一种共价键性很强的化合物,其自扩散系数非常小,导致其可烧结性很差,通过添加助烧剂后能够使SiC在较低的温度发生烧结。
优选的,所述硼粉的粒径为10-20μm。
通过采用上述技术方案,B能够在反应过程中与硅片中的N反应生成BN,从而促进反应烧结,有利于生成致密的高导热碳化硅材料。
第二方面,本申请提供一种高导热碳化硅材料的制备方法,采用如下的技术方案:
一种高导热碳化硅材料的制备方法,包括如下制备步骤:
S1、根据配方比例称取各原料,加水混合均匀,得到料浆;
S2、将S1中的料浆经喷雾干燥造粒,得到粒料;
S3、将S2中的粒料压制成型,得到素坯;
S4、将S3中的素坯烘焙成型,然后进行加工;
S5、真空烧结,经自然冷却后得到高导热碳化硅材料。
通过采用上述技术方案,采用上述工艺制得的高导热碳化硅材料具有良好的热传导性能,且由于机械密封环在工作时会因摩擦而产生大量热量,当应用上述工艺制备得到的高导热碳化硅材料应用到机械密封环上时,密封环所产生的热量能够得到有效的散发,使得机械密封环具有较好的散热性能,从而提高了机械密封环的使用寿命。
其中,喷雾造粒能够提高素坯的均匀性和压制成型后的密度,利用喷雾造粒技术制得的粒料具有良好的流动性能和化学均匀性。碳化硅属于瘠性原料,在不加粘结剂的情况下难以成型,而在有粘结剂的情况下也容易出现内部裂纹、坯体密度不均等缺陷,严重影响最终性能和产品的稳定性,通过喷雾造粒可改善其成型性,同时也有利于大规模生产的产品性能稳定。
优选的,S3中,粒料压制成型的压力为120-150MPa。
通过采用上述技术方案,120-150MPa的压力条件下制得的素坯具有良好的致密性。
优选的,S4中,在素坯上方放置硅片再进行烘焙成型。
通过采用上述技术方案,素坯中含有大量空隙,烘焙成型时在素坯上方放置硅片能够使得硅片中的硅渗透至空隙中,从而增加高导热碳化硅材料的致密性,同时Si会与C反应生成新的SiC,从而提高产品强度,增加断裂韧性。
优选的,S5中,真空烧结的温度为1600-1650℃,升温速度为4℃/min,保温时间为1-3h。
通过采用上述技术方案,1600-1650℃的温度范围内进行真空烧结,能够得到致密的高导热碳化硅材料。
4℃/min的升温速度能够使助烧剂和粘结剂在烧结过程中被热解或脱除,水溶性酚醛树脂的热分解反应完全。
综上所述,本申请具有以下有益效果:
1、由于本申请采用碳化硅和金刚石的复合材料,由于金刚石的添加在提高了导热系数的同时增加了硬度,从而使高导热碳化硅材料具有良好的导热性能和机械性能。
2、本申请中优选采用在原料中添加石墨粉,由于碳化硅与石墨粉在反应过程中能够经过加热与液态Si反应生成β-SiC,从而提高产品强度,从而起到增加断裂韧性的效果;
3、本申请中优选采用在原料中硼粉,由于B能够在反应过程中与硅片中的N反应生成BN,从而促进反应的烧结;
4、本申请的方法,粒料通过冷压机压制成型,相较于热压机而言,节省了能耗,从而降低了生产成本。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
本申请中的水溶性酚醛树脂、硼粉和明胶均选自上海麦克林生化科技有限公司,其中,硼粉的粒径为10-20μm;硅片选自哈尔滨特博科技有限公司。
实施例1
一种高导热碳化硅材料的制备方法,包括如下制备步骤:
S1、按重量称取各原料,包括:碳化硅700g,金刚石80g,石墨粉20g,水溶性酚醛树脂100g,明胶20g,硼粉15g和75g硅片;
S2、将S1中各原料投入球磨机中,并加入1500g水混合均匀,得到料浆;
S3、将S2中的料浆经喷雾干燥工艺进行造粒,得到粒料;
S4、使用冷压机,将S3中的粒料在150MPa的压力条件下压制成型,得到素坯;
S5、将S4中的素坯烘焙成型,烘焙成型时素坯上方放置有硅片,然后进行加工;
S6、在1600℃的温度下进行真空烧结,升温速度为4℃/min,保温时间为3h,再经自然冷却后得到高导热碳化硅材料。
实施例2-5
实施例2-5中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于高导热碳化硅材料的原料组成及用量不同,具体如表1和表2所示:
表1 实施例1-5中高导热碳化硅材料的原料组成及用量
表2 实施例1-5中高导热碳化硅材料制备方法的各参数
实施例6
本实施例中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于S3中,烘焙成型时素坯上方未放置硅片。
实施例7
本实施例中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于S3中压制成型时的压力100MPa。
实施例8
本实施例中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于S5中真空烧结的温度为1550℃,保温3h。
实施例9
本实施例中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于S5中真空烧结的温度为1700℃,保温3h。
对比例1
本实施例中高导热碳化硅材料的制备方法与实施例1相同,区别仅在于原料中不添加金刚石。
性能检测试验
洛氏硬度(HRC):按照GB/T 230.1—2009《金属材料 洛氏硬度试验》;
样品密度:采用QB/T 1010-2015《陶瓷材料、颜料真密度的测定方法》;
导热系数:采用GB/T 2480-2008《普通磨料 碳化硅》;
裂缝概率:观察50个产品的表面是否出现裂缝,计算出现裂缝的概率;
渗漏测试:将材料制成10cm×10cm×2cm的方块,液压管端面与方块表面进行密封,对液压管内的水施加10MPa的压力,静置24h,观察方块另一侧表面是否出现渗漏现象。
表3 实施例1-9和对比例1的试验结果
结合实施例1-5并结合表3可以看出,实施例1-5中高导热碳化硅材料的导热系数均大于纯碳化硅材料的导热系数,且导热系数增加了近1倍,说明本申请制得的高导热碳化硅材料具有良好的导热性能,由实施例1-5中任一高导热碳化硅材料制得的机械密封环均具有良好的散热性能,能够在工作时将产生的热量及时散失,从而延长了机械密封环的使用寿命。同时,纯碳化硅材料的硬度为HRC91,而实施例1-5中高导热碳化硅材料的硬度提升至HRC95左右。
结合实施例1和实施例6并结合表3可以看出,实施例6在烘焙成型时未在素坯上方放置硅片,所测得的高导热碳化硅材料密度小于实施例1测得的高导热碳化硅材料密度,说明烘焙成型过程中将硅片放置在素坯上方,硅片中的硅会渗透至素坯中的空隙,从而增加高导热碳化硅材料的致密性。
结合实施例1和实施例7并结合表3可以看出,实施例7中高导热碳化硅材料的密度小于实施例1中高导热碳化硅材料的密度,实施例7中高导热碳化硅材料的抗折强度小于实施例1中高导热碳化硅材料的抗折强度,说明压制成型时压力小于120MPa,不利于制得致密的高导热碳化硅材料,制得的高导热碳化硅材料力学性能也会有所下降。
结合实施例1和实施例8-9并结合表3可以看出,实施例8烧结温度为1550℃,小于1600℃,在此温度下烧结制得的高导热碳化硅材料,其密度较实施例1有所下降;实施例9烧结温度为1700℃,大于1650℃,其各项参数较实施例1相比,无明显差别。
结合实施例1和对比例1并结合表3可以看出,对比例1中原料未添加金刚石,其制得的高导热碳化硅材料硬度明显下降,说明金刚石的添加有利于提高高导热碳化硅材料的力学性能;同时,对比例1中高导热碳化硅材料的导热系数小于实施例1中高导热碳化硅材料的导热系数,说明金刚石的添加有利于提高高导热碳化硅材料的导热性能;由于金刚石的密度小于碳化硅的密度,所以对比例1的密度小于实施例1的密度。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (8)
1.一种高导热碳化硅材料,其特征在于,所述高导热碳化硅材料由以下重量份数的原料组成:碳化硅65-75份,金刚石3-10份,石墨粉18-22份,粘结剂1-5份,助烧剂2-10份、硼粉1-3份和硅片5-15份。
2.根据权利要求1所述的一种高导热碳化硅材料,其特征在于:所述粘结剂为聚乙烯醇、乙基羟甲基纤维素和明胶中的至少一种。
3.根据权利要求1所述的一种高导热碳化硅材料,其特征在于:所述助烧剂为水溶性酚醛树脂和丙烯酸中的其中一种。
4.根据权利要求1所述的一种高导热碳化硅材料,其特征在于:所述硼粉的粒径为10-20μm。
5.如权利要求1-4任一项所述的一种高导热碳化硅材料的制备方法,其特征在于,包括如下制备步骤:
S1、根据配方比例称取各原料,加水混合均匀,得到料浆;
S2、将S1中的料浆经喷雾干燥造粒,得到粒料;
S3、将S2中的粒料压制成型,得到素坯;
S4、将S3中的素坯烘焙成型,然后进行加工;
S5、真空烧结,经自然冷却后得到高导热碳化硅材料。
6.根据权利要求5所述的一种高导热碳化硅材料的制备方法,其特征在于:S3中,粒料压制成型的压力为120-150MPa。
7.根据权利要求5所述的一种高导热碳化硅材料的制备方法,其特征在于:S4中,在素坯上方放置硅片再进行烘焙成型。
8.根据权利要求5所述的一种高导热碳化硅材料的制备方法,其特征在于:S5中,真空烧结的温度为1600-1650℃,升温速度为4℃/min,保温时间为1-3h。
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