CN102596802A - 用于制备碳化硅粉体的系统和方法 - Google Patents
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Abstract
本发明公开了一种高纯碳化硅粉体的制备方法和系统。即,本发明的高纯碳化硅粉体的制备方法包括:在混合器中制备由硅源和碳源组成的混合物的步骤;和通过在大于0.03托且等于和小于0.5托的真空度和在等于或大于1300℃且等于和小于1900℃的温度下加热所述混合物来合成碳化硅(SiC)粉体的步骤。
Description
技术领域
本发明涉及用于制备碳化硅粉体的方法和系统。
背景技术
SiC(碳化硅)和硼(B)是具有较高拉伸比的增强材料。虽然Al2O3是氧化剂陶瓷的代表,但SiC广泛用作非氧化剂陶瓷的代表性材料。SiC纤维,作为形成陶瓷和金属复合材料的增强材料,在其使用方面被大力开发,而硼纤维主要用作高端性能的环氧增强材料。
特别是,在仅有的比其它增强材料更昂贵的成本问题被解决的情况下,具备优异物理性能的SiC肯定是大量使用的增强材料。
SiC作为复合材料,是陶瓷领域中最基本的碳化物之一。
在碳化硅中,存在具有立方晶体结构的β-相和具有六方晶体结构的α-相。β-相在1400-1800℃的温度范围下是稳定存在的,而α-相在高于2000℃下形成。
SiC的分子量为40.1,它的比重为3.21,且在大约2500℃或大于2500℃下分解。
自从U.S.A.G.E.′s Prochazka于20世纪70年代通过添加硼和碳首先成功完成无压烧结后,碳化硅(SiC)具有相当大的高温强度,在耐磨损、抗氧化、防腐蚀、抗蠕变等方面具有优异的性能,从而作为高温结构材料引起注意,并且是目前广泛使用的高级陶瓷材料,用于例如机械密封、轴承、各种喷嘴、高温切削工具、防火板、磨料、炼钢中的还原剂以及避雷器。
在制备这样的SiC粉体的现有技术中,存在Acheson法、直接反应法、液体聚合物裂解法和高温自蔓延合成法等。
这些常规技术通过混合固态硅源(例如,SiO2和Si)和碳源(例如碳和石墨)并在1350℃~2000℃下进行热处理而制备碳化硅。这些常规技术伴随有SiC粉体回收率的问题,以及具有在纯度方面的限制和相对较高的复合温度。
此外,因为碳化硅难以批量生产且需要例如分类清洗的额外处理,所以由于花费的较长的制备时间,存在所制备的碳化硅粉体的成本昂贵的弱点。
因此,像我们国家一样在从国外进口全部量的框架中,极度需要以低成本制备碳化硅粉体的制备方法,以及如此制得的、高纯度和均匀的碳化硅粉体。
发明内容
技术问题
本发明意在提供一种能够便宜地和容易地制备碳化硅粉体的高纯碳化硅粉体的制备方法和系统。
另外,本发明要提供一种制备碳化硅粉体的方法,所述方法可以减少制备碳化硅粉体所需的反应能量,以降低热处理温度、缩短处理时间同时得到较高回收率。
技术方案
本发明涉及一种碳化硅粉体的制备方法,其特征在于所述方法包括以下步骤:步骤(a),在混合器中制备由硅源和碳源组成的混合物;和步骤(b),通过在大于0.03托且等于和小于0.5托的真空度和等于或大于1300℃且等于和小于1900℃的温度下加热所述混合物来合成碳化硅(SiC)粉体。
另外,在所述步骤(a)中,所述硅源和所述碳源的质量比特征在于等于和大于1∶1且等于和小于4∶1。
在本说明书中,所述步骤(a)中的硅源选自热解法二氧化硅、硅溶胶、硅凝胶、微粉二氧化硅和石英粉中的一种和多种。
另外,所述碳源特征在于选自如下中的一种和多种:包括炭黑、碳纳米管、富勒烯(fullerene)、酚树脂、franc树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚丙烯腈、聚乙烯醇和聚乙酸乙烯酯(poly acetic acid vinyl)的单体,预聚物,纤维素,制成的糖,沥青,以及焦油。
此外,所述步骤(b)的加热温度特征在于等于或大于1600℃且等于和小于1900℃。
另外,所述步骤(b)的加热时间特征在于为3小时。
特别是,在所述步骤(a)和所述步骤(b)之间,所述碳化硅粉体的制备方法还包括加热所述混合物并使该混合物中含有的碳源碳化的步骤。
此处,所述碳化步骤的特征在于在等于或大于700℃且等于和小于1200℃的温度下进行碳化。
另外,所述碳化步骤的特征在于在等于或大于900℃且等于和小于1100℃的温度下进行碳化。
另外,本发明的碳化硅粉体的制备系统,特征在于包括混合器,用于制备由硅源和碳源组成的混合物;和密封坩埚,用于通过在等于或大于0.03托且等于和小于0.5托的真空度和在等于和大于1300℃且等于和小于1900℃的温度下加热所述混合物来合成碳化硅(SiC)。
另外,所述硅源和所述碳源的质量比特征在于等于和大于1∶1且等于和小于4∶1。
另外,所述硅源是热解法二氧化硅,以及所述碳源是炭黑。
另外,所述坩埚的加热温度特征在于等于或大于1600℃且等于和小于1900℃。
另外,所述加热时间特征在于为30分钟~5小时。
特别是,所述碳化硅粉体的制备系统还包括碳化器,用于通过加热所述混合物使该混合物中含有的碳源碳化。
另外,所述碳化器特征在于在等于和大于700℃且等于和小于1200℃的温度下进行碳化。
另外,所述碳化器特征在于在等于和大于900℃且等于和小于1100℃的温度下进行碳化。
此外,本发明涉及一种碳化硅粉体的制备方法,所述方法包括以下步骤:步骤(a),通过在混合器中混合SiO粉末和碳源来制备碳化硅原料混合物;和步骤(b),通过在坩埚中在等于和大于1,400℃且等于和小于1,700℃的温度下热处理所述混合物30分钟和多于30分钟且7小时和少于7小时来制备碳化硅粉体。
另外,所述步骤(a)的碳源特征在于为炭黑。
另外,在所述步骤(a)中,碳对硅的混合比特征在于为等于和大于1.3且等于和小于1.8。
另外,所述步骤(a)使用球磨机作为混合器,其特征在于通过混合SiO、碳源和用于球磨机的球来制备碳化硅混合物。
特别是,在所述步骤(a)和所述步骤(b)之间,所述方法还包括步骤(1):通过使用筛网过滤出用于球磨机的球来回收碳化硅混合物。
另外,在所述步骤(a)和所述步骤(b)之间,所述方法还包括步骤(2):在石墨坩埚中测量回收的混合物。
另外,在所述步骤(b)中的坩埚材料是石墨,其特征在于在内部空间形成真空或填充惰性气体。
有益效果
与现有的碳化硅粉体制备方法相比,本发明可以在低压和低温下制备,可以节省处理成本并易于得到高纯度碳化硅粉体。
本发明可以在合成碳化硅粉体中的热处理工序中降低温度和缩短时间,且相比于一般硅化合物使用过程,提高了碳化硅粉体的回收率。
附图说明
图1是根据本发明的一个优选实施方案的碳化硅粉体制备方法的框图;
图2是根据本发明的一个优选实施方案的碳化硅粉体制备系统的构成框图;以及
图3是根据本发明的另一个优选实施方案的碳化硅粉体制备方法的流程图。
具体实施方式
在下文中,将考虑附图详细说明根据一个优选实施方案的碳化硅粉体的制备方法和系统。然而,在描述该实施方案中,在确定使得本发明的实质必然不模糊的情形下,将省略掉关于相关众所周知的功能或结构的具体描述。
图1是根据本发明的一个优选实施方案的碳化硅粉体制备方法的框图。
参照图1,首先准备硅源和碳源,特别合意的是准备热解法二氧化硅作为硅源和炭黑作为碳源(S1)。然而,所述硅源和碳源限于那些已提到的,但硅溶胶、SiO2(硅凝胶)、微粉二氧化硅和石英粉可以用作硅源。
另外,作为碳源,可以使用固体碳,例如碳纳米管,富勒烯;或具有较高残碳率的有机化合物,例如,单体或预聚物,比如酚树脂、franc树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚丙烯腈、聚乙烯醇和聚乙酸乙烯酯,纤维素,制成的糖,沥青,焦油,以及它们的混合物。
而后,将这样的硅源和碳源混合。特别是,将40g作为硅源的热解法二氧化硅和18g作为碳源的炭黑混合(S2)。此处,在使用固体碳源的情形中,硅源和碳源的质量比合意的是等于和大于1∶1且等于和小于4∶1。
另外,有机碳源的使用需要具有超过固体碳源约2倍质量的碳源,但基于随后的碳化工序中得到的碳产率,液体碳源可能有些差别。然后,加热混合有硅源和碳源的混合物,从而使该混合物中含有的碳源碳化(S3)。
所述碳化过程合意的是在等于和大于700℃且等于和小于1200℃的温度下进行。另外,更合意的是使碳化过程的温度保持在等于和大于900℃且等于和小于1100℃,并且在碳源不是有机碳材料的情形中,可以省略所述碳化过程。
随后,所述混合物在大于0.03托且等于和小于0.5托的真空度下和在等于或大于1300℃且等于和小于1900℃的温度下加热,以合成碳化硅(SiC)粉体(S4)。
此处,加热时间合意的是30分钟~5小时,但不必须限于此。
另外,加热温度更合意的是等于或大于1600℃且等于和小于1900℃。另外,合成工艺条件合意的是具有1托的真空度,且更合意的是在0.1托和小于0.1托的真空气氛下进行热处理。
然而,由于下面的原因真空度为0.03托和小于0.03托的情形是不期望的。在大批量生产设备中大量消耗机械负载;需要额外的设备;设备难以维护;以及附随成本高。
通过使用本发明的这种工艺,可以以低成本制备高纯度碳化硅粉体。在下面表1中显示了与使用现有方法的情形对比的这种效果。
表1
参照图1,对比例表示以现有方式制备碳化硅粉体的情形。且,第一实施例和第二实施例是使用根据本发明的制备方法制备碳化硅粉体的情形。此处,在所有情形中的共同条件是选择40g平均直径为40nm的热解法二氧化硅作为硅源和18g平均直径为20nm的炭黑作为碳源以进行混合过程,以及省略碳化过程。
另外,作为区别,所述对比例显示在坩埚中氩气(Ar)环境下,在1700℃的温度下合成3小时的一个情形。另一方面,第一实施例是在坩埚中在等于和大于0.1托且等于和小于0.5托的真空度下,在1700℃下合成3小时的实施例,以及第二实施例是在等于和大于0.1托且等于和小于0.5托的真空度下,在1600℃下合成3小时的实施例。
如试验结果所示,第一实施例和第二实施例中的杂质含量显著小于对比例。因此,使用本发明通过采用真空状态代替使用氩气,可以节省制备成本和制得含有非常少的杂质的高纯碳化硅粉体。
图2是根据本发明的一个优选实施方案的碳化硅粉体制备系统的构成框图。
碳化硅粉体制备系统100包括混合器110、坩埚120和碳化器130。混合器使硅源和碳源混合以制备由硅源和碳源组成的混合物。此处,所述硅源和碳源可以选自图1中描述的各个种类。特别是,硅源和碳源的质量比合意的是等于和大于1∶1且等于和小于4∶1。另外,碳化器130与混合器110和坩埚120相连,且使混合物中含有的碳源碳化。另外,在碳化器130中的碳化温度优选为等于和大于700℃且等于和小于1200℃,更优选在等于和大于900℃且等于和小于1100℃下碳化。特别是,在混合物的碳源不是有机碳材料的情形中可以省略碳化器130,且在此情形中,混合物从混合器110中直接移至坩埚120中。
另外,坩埚120在大于0.03托且等于和小于0.5托的真空度下和在等于和大于1300℃且等于和小于1900℃的温度下对混合物进行加热,以合成碳化硅(SiC)粉体。具体地,坩埚的加热温度更合意的是等于和大于1600℃且等于和小于1900℃。另外,在坩埚130中的加热时间合意的是3小时。
上述碳化硅粉体制备系统可以制备低成本和高纯度的碳化硅粉体。
图3是根据本发明另一个优选实施方案的碳化硅粉体制备方法的流程图。
参照图3,准备SiO粉末和炭黑(S1)。
SiO是SiO2和C的过程中物质(in-process material)。此处,炭黑用作碳源,但不必须限于此。例如,可以使用固体碳,例如碳纳米管、富勒烯或具有较高残碳率的有机化合物,具体而言,所述有机化合物为例如酚树脂、franc树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚丙烯腈、聚乙烯醇和聚乙酸乙烯酯的单体或预聚物,纤维素,制成的糖,沥青,焦油,以及它们的混合物。
将这样制得的SiO粉末和炭黑粉末混入混合器中,即,球磨机(S2)中。此处,当C∶Si之比是2∶1时,SiO和C的混合比理论上是最理想的。然而,因为SiO在气化中实际上被挥发,所以C∶Si之比合意的是等于和大于1.3∶1且等于和小于1.8∶1。另外,为了防止在球磨机中混合的碳化硅粉体结块,将用于球磨机的球一起混合。这种用于球磨机的球可以使用尼龙球、聚氨酯球和特氟龙球等。
随后,使用筛网回收球磨机中混合的碳化硅原料粉末(S3)。此处,筛网可以使用金属筛网或聚合物筛网。使用这种筛网过滤出用于球磨机的球且可以仅回收碳化硅粉体。
接下来,在石墨坩埚中测量在S3中过滤出的碳化硅粉体原料混合物(S4)。测量的原因是通过测量进入加热炉的最终碳化硅原料的量来得出制备效率。
然后,通过在等于和大于1400℃且等于和小于1700℃的温度下在石墨炉中加热30分钟和大于30分钟且7小时和小于7小时来合成碳化硅粉体(S5)。
这种石墨炉中发生的碳化硅粉体的合成步骤如下面反应1所示。
[化学反应1]
SiO+C→Si+CO
Si+C→SiC
-----------------------
SiO+2C→SiC+CO
在此种情形中,石墨炉中的内部形成真空或填充惰性气体(例如,氩气(Ar)和氢气(H),等)。
此后,最终回收碳化硅粉体(S6)。
在下表2中显示出上述依据本发明的改进事实。
表2
对比例 | 实施例 | |
温度 | 1650℃ | 1400℃ |
时间 | 5 | 3 |
回收率 | 30% | 53% |
颗粒大小(D50) | 1.4μm | 1.3μm |
参照表2,对比例表示现有技术,对于硅化合物使用SiO2,以及对于碳化合物使用炭黑。这些混合物由2.5∶1(小于3∶1)的比例组成,这是在球磨机中存在的SiO2和C的理论混合比。另外,在坩埚中在1650℃下热处理5小时后,通过XRD(X射线衍射)确认SiC晶体峰。
另外,根据本发明的制备方法,实施例使用SiO作为硅化合物和炭黑作为碳化合物。这种C∶Si的混合物在球磨机中以C∶Si为1.8∶1的比例进行混合。另外,在坩埚中在1400℃下热处理3小时后,通过XRD确认SiC晶体峰。
如试验结果所示,本发明已将加热温度降低了200℃(从1650℃到1400℃)且将时间缩短了2小时。另外,碳化硅粉体的回收率从30%逐渐升高到50%,而且在颗粒大小(D50)方面,可以制得从1.4μm到1.3μm的更细粉体。
因此,由于更有效率的工艺,可以制得更高回收率和细的碳化硅粉体。
如上所述,本发明已经对于具体实施方案进行了详细描述。然而,在不背离本发明的范围下可以做出各种改变。本发明技术的精神不应该以限制性意义理解成本发明描述的实施方案,但必须限定成权利要求以及这种权利要求的等同形式。
工业实用性
本发明可以提供能够通过低压和低温制备且能够节省工艺成本的碳化硅粉体制备方法和系统。
Claims (13)
1.一种碳化硅粉体的制备方法,其特征在于:
步骤(a),在混合器中制备由硅源和碳源组成的混合物;和
步骤(b),通过在大于0.03托且等于和小于0.5托的真空度和在等于或大于1300℃且等于和小于1900℃的温度下加热所述混合物来合成碳化硅(SiC)粉体。
2.根据权利要求1所述的方法,其中,在所述步骤(a)中,所述硅源和所述碳源的质量比等于和大于1∶1且等于和小于4∶1。
3.根据权利要求2所述的方法,其特征在于,所述步骤(a)中的硅源选自热解法二氧化硅、硅溶胶、硅凝胶、微粉二氧化硅和石英粉中的一种和多种,其中所述碳源选自如下中的一种和多种:包括炭黑、碳纳米管、富勒烯、酚树脂、franc树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚丙烯腈、聚乙烯醇和聚乙酸乙烯酯的单体,预聚物,纤维素,制成的糖,沥青,以及焦油。
4.根据权利要求1所述的方法,其特征在于,在所述步骤(a)和所述步骤(b)之间,所述方法还包括加热所述混合物并使该混合物中含有的碳源碳化。
5.根据权利要求4所述的方法,其特征在于,所述碳化步骤包括在等于或大于700℃且等于和小于1200℃的温度下进行碳化。
6.一种碳化硅粉体的制备方法,其特征在于:
步骤(a),通过在混合器中混合SiO粉末和碳源来制备碳化硅原料混合物;和
步骤(b),通过在坩埚中在等于和大于1,400℃且等于和小于1,700℃的温度下热处理所述混合物30分钟和多于30分钟且7小时和小于7小时,来制备碳化硅粉体。
7.根据权利要求6所述的方法,其特征在于,在所述步骤(a)中,所述碳源为炭黑。
8.根据权利要求7所述的方法,其特征在于,在所述步骤(a)中,碳(C)对硅(Si)的混合比为等于和大于1.3且等于和小于1.8。
9.根据权利要求1所述的方法,其特征在于,在所述步骤(a)和所述步骤(b)之间,所述方法还包括:步骤(1),通过使用筛网过滤出用于球磨机的球来回收碳化硅混合物;和
步骤(2),在石墨坩埚中测量回收的混合物,其中所述步骤(a)使用球磨机作为混合器,其特征在于通过混合SiO、碳源和用于球磨机的球来制备碳化硅混合物的步骤。
10.根据权利要求9所述的方法,其特征在于,在所述步骤(b)中的加热炉材料是石墨,通过在内部空间形成真空或填充惰性气体。
11.一种碳化硅粉体的制备系统,其特征在于:
混合器,用于制备由硅源和碳源组成的混合物;和
密封坩埚,用于通过在等于或大于0.03托且等于和小于0.5托的真空度和在等于和大于1300℃且等于和小于1900℃的温度下加热所述混合物来合成碳化硅(SiC)。
12.根据权利要求11所述的系统,其特征在于,所述硅源和所述碳源的质量比等于和大于1∶1且等于和小于4∶1。
13.根据权利要求11所述的系统,其特征在于,所述硅源选自热解法二氧化硅、硅溶胶、硅凝胶、微粉二氧化硅和石英粉中的一种和多种,其中所述碳源特征在于选自如下中的一种和多种:包括炭黑、碳纳米管、富勒烯、酚树脂、franc树脂、二甲苯树脂、聚酰亚胺、聚氨酯、聚丙烯腈、聚乙烯醇和聚乙酸乙烯酯的单体,预聚物,纤维素,制成的糖,沥青,以及焦油。
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WO2017180083A1 (ru) * | 2016-04-15 | 2017-10-19 | Андрей ЦЫБА | Способ промышленного производства нанопорошков sic и нанокомпозита sio-c высокого качества и комплекс для его реализации |
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CN113666375B (zh) * | 2021-09-06 | 2023-10-27 | 常州大学 | 一种绿色制备高比表面积β-碳化硅的方法 |
Also Published As
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WO2011025285A2 (en) | 2011-03-03 |
JP2013503099A (ja) | 2013-01-31 |
WO2011025285A3 (en) | 2011-07-14 |
EP2470473A4 (en) | 2014-10-08 |
US20120201735A1 (en) | 2012-08-09 |
EP2470473A2 (en) | 2012-07-04 |
JP5525050B2 (ja) | 2014-06-18 |
EP2470473B1 (en) | 2017-12-20 |
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