CN114685170A - 微波闪烧合成碳化硅的方法 - Google Patents
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 51
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000010304 firing Methods 0.000 title claims abstract description 42
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Abstract
本发明涉及一种微波闪烧合成碳化硅的方法，首先，将硅源和碳源均匀混合，之后，将得到的混合粉体直接置于微波烧结炉中进行微波烧成，或者，将混合后的粉体先进行预成型，之后再置于微波烧结炉中进行微波烧成；微波烧成的过程包括：将微波烧结炉的输入功率升至3KW以上，温度迅速上升到设定温度后，不保温，立即结束烧制，完成微波烧成，合成碳化硅；所述的设定温度不小于600℃。本发明借助微波加热快速、节约能源且保护环境的优势，将硅源和碳源混合后直接在高微波输入功率下一分钟内实现碳化硅的合成，效率极高，且通过本发明方法可制得纯度高的α‑SiC。
Description
技术领域
本发明涉及无机非金属材料制备技术领域，具体涉及一种微波闪烧合成碳化硅的方法。
背景技术
碳化硅(SiC)陶瓷具有优良的高温力学性能、抗氧化性强、耐磨损性好、热稳定性佳、热膨胀系数小、热导率大、弹性模量高，高温电性能优良、硬度高以及抗热震和耐化学腐蚀等优良性能，在汽车、机械化工、环境保护、空间技术、信息电子、能源等领域有着日益广泛的应用，己经成为一种在很多工业领域性能优异的其他材料不可替代的结构陶瓷，并日益受到人们的重视。
SiC粉料的合成方法主要分为三种：
(1)固相法，包括粉末煅烧法、碳热还原法、自蔓延高温合成法和机械粉碎法；
(2)液相法，包括溶胶-凝胶法和聚合物热分解法；
(3)气相法，包括化学气相沉积法、等离子体法和激光诱导法等。
其中，固相法由于成本低廉、原料易获得等优势，已广泛用于工业化生产。然而，碳化硅由于存在极强的共价键，因此，目前，碳化硅的合成需要在高温下实现(普遍在1400～2700℃)，且合成周期较长，普遍在5～100小时，造成了大量的能源浪费。
由此可见，上述现有的碳化硅的制备方法显然仍存在有不便与缺陷，而亟待加以进一步改进，但长久以来一直未见适用的方法被报道。本发明人基于从事此类产品设计制造多年丰富的实务经验及专业知识，积极加以研究创新，以期创设一种微波闪烧合成碳化硅的方法，能够改进一般现有合成碳化硅需要在高温下完成以及合成周期长的缺陷，经过不断的研究、设计，并经过反复试作样品及改进后，终于创设出确具实用价值的本发明。
发明内容
针对现有技术存在的缺陷，本发明提供一种微波闪烧合成碳化硅的方法，借助微波加热快速、节约能源且保护环境的优势，将硅源和碳源混合后直接在高微波输入功率下一分钟内实现碳化硅的合成。
本发明的发明目的是通过以下技术方案来实现的，依据本发明提出的一种微波闪烧合成碳化硅的方法，具体包括以下步骤：
(1)将硅源、碳源均匀混合；
(2)将混合后的粉体直接置于微波烧结炉中进行微波烧成，或者，将混合后的粉体先进行预成型，之后再置于微波烧结炉中进行微波烧成；微波烧成的过程包括：将微波烧结炉的输入功率升至3KW以上，温度迅速上升到设定温度后，不保温，立即结束烧制，完成微波烧成，合成碳化硅；所述的设定温度不小于600℃。
前述的微波闪烧合成碳化硅的方法，其中，步骤(1)中所述的硅源包括但不限于硅粉、正硅酸乙酯、石英砂、白炭黑，硅溶胶等中的一种或多种。
前述的微波闪烧合成碳化硅的方法，其中，步骤(1)中所述的碳源包括但不限于工业煤、石墨、活性炭、石油焦等中的一种或多种。
前述的微波闪烧合成碳化硅的方法，其中，步骤(1)中碳源和硅源中碳硅摩尔比为0.5～10：1；混料方式包括但不限于球磨法、研磨法、机械搅拌等。
前述的微波闪烧合成碳化硅的方法，其中，步骤(2)中的成型方式包括但不限于干压成型、等静压成型、溶胶凝胶成型等。
前述的微波闪烧合成碳化硅的方法，其中，步骤(2)中微波烧成时输入功率为3KW～10KW，加热频率为915MHz或2450MHz。
前述的微波闪烧合成碳化硅的方法，其中，按照上述方法最终制备得到α-SiC。
前述的微波闪烧合成碳化硅的方法，其中，所制备的α-SiC晶体发育良好，为典型的六方结构。
前述的微波闪烧合成碳化硅的方法，所制备的α-SiC在制备半导体材料、功能陶瓷、高级耐火材料等领域具有潜在的巨大应用价值。
本发明与现有技术相比具有明显的优点和有益效果。借由上述技术方案，本发明一种微波闪烧合成碳化硅的方法可达到相当的技术进步性及实用性，并具有广泛的利用价值，其至少具有下列优点：
本发明借助微波加热快速、节约能源且保护环境的优势，将硅源和碳源混合后直接进行微波烧成，或者混合后先预成型再进行微波烧成，在高微波输入功率下，一分钟内实现碳化硅的合成，其效率极高，极大地加快了制备α-SiC的速率，缩短了制备周期，相比现有技术的烧结温度(普遍在1400～2700℃范围内)，本发明的烧结温度显著降低，在600～1100℃范围内，一分钟内即可完成α-SiC的制备，且所制备的α-SiC具有非常高的纯度，纯度>99％，该α-SiC可以应用于制备半导体材料，功能陶瓷、高级耐火材料等。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，而可依照说明书的内容予以实施，并且为了让本发明的上述和其他目的、特征和优点能够更明显易懂，以下特举较佳实施例，并配合附图，详细说明如下。
附图说明
图1为实施例1中制备的碳化硅的扫描电镜图；
图2为实施例1中制备的碳化硅的XRD图谱。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合具体实施例以及附图，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部实施例。基于本发明的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明所提供的一种微波闪烧合成碳化硅的方法，具体包括以下步骤：
(1)将硅源、碳源均匀混合，混合的方式包括但不限于球磨法混合、研磨法混合、机械搅拌混合等。
硅源可以选用硅粉、正硅酸乙酯、石英砂、白炭黑，硅溶胶等中的一种或多种。
碳源可以选用工业煤、石墨、活性炭、石油焦等中的一种或多种；碳硅摩尔比为0.5～10：1。
(2)将混合后的粉体直接置于微波烧结炉中进行微波烧成，或者，将混合后的粉体先通过干压成型、等静压成型、溶胶凝胶成型等成型方法进行预成型，之后再置于微波烧结炉中进行微波烧成。
微波烧成的过程包括：将微波烧结炉的输入功率升至3KW以上，温度迅速上升到设定温度后，不保温，立即结束烧制，完成微波烧成，合成α-SiC；所述的设定温度不小于600℃。
优选地，微波烧成时输入功率为3KW～10KW，加热频率为915MHz或2450MHz。
实施例1：
选取粒径为2000目的碳粉为碳源，粒径为1000目的硅粉为硅源，碳硅摩尔比为1:1，以酒精为研磨介质，以300r/min球磨12h进行粉体混合；之后，将混合粉体置于微波烧结炉中，将输入功率调整到5KW，加热频率为2450MHz，样品迅速升温到800℃后，不保温，立即结束烧制，得到碳化硅。
图1是本实施例所制备的碳化硅的扫描电镜图，由图1可知，所制备的碳化硅晶体发育良好，为典型的六方结构。
图2是本实施例所制备的碳化硅的XRD图谱，由图2可知：制备的样品为纯α-SiC相。
实施例2：
选取粒径为1000目的活性炭为碳源，粒径为325目的硅粉为硅源，碳硅摩尔比为2:1，以酒精为研磨介质，以300r/min球磨24h进行粉体混合；之后，将混合粉体置于微波烧结炉中，将输入功率调整到6KW，加热频率为2450MHz，样品迅速升温到700℃后，不保温，立即结束烧制，得到碳化硅。
实施例3：
选取粒径为325目的石油焦为碳源，粒径为2000目的石英砂为硅源，碳硅摩尔比为3:1，以酒精为研磨介质，以300r/min球磨24h进行粉体混合；之后，将混合粉体利用等静压机在20MPa压力下保压2min得到坯体。将坯体置于微波烧结炉中，将输入功率调整到4KW，加热频率为2450MHz，样品迅速升温到900℃后，不保温，立即结束烧制，得到碳化硅。
实施例4：
选取粒径为1000目的石墨为碳源，粒径为1000目的硅粉为硅源，碳硅摩尔比为2:1，以酒精为研磨介质，以300r/min球磨24h进行粉体混合；之后，将混合粉体利用干压机在50MPa压力下保压1min得到坯体。将坯体置于微波烧结炉中，将输入功率调整到7KW，加热频率为915MHz，样品迅速升温到1000℃后，不保温，立即结束烧制，得到碳化硅。
实施例5：
选取粒径为1000目的石墨为碳源，粒径为1000目的硅粉为硅源，碳硅摩尔比为1:1，以酒精为研磨介质，以300r/min球磨24h进行粉体混合；之后，将混合粉体利用等静压机在10MPa压力下保压5min得到坯体。将坯体置于微波烧结炉中，将输入功率调整到3KW，加热频率为2450MHz，样品迅速升温到650℃后，不保温，立即结束烧制，得到碳化硅。
以上所述仅是本发明的具体实施例，并非对本发明作任何形式上的限制，本发明还可以根据以上结构和功能具有其它形式的实施例，不再一一列举。因此，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。
Claims (10)
1.微波闪烧合成碳化硅的方法，其特征在于包括以下步骤：
(1)将硅源、碳源均匀混合；
(2)将混合后的粉体直接置于微波烧结炉中进行微波烧成，或者，将混合后的粉体先进行预成型，之后再置于微波烧结炉中进行微波烧成；微波烧成的过程包括：将微波烧结炉的输入功率升至3KW以上，温度迅速上升到设定温度后，不保温，立即结束烧制，完成微波烧成，合成碳化硅；所述的设定温度不小于600℃。
2.如权利要求1所述的微波闪烧合成碳化硅的方法，其特征在于步骤(1)中所述的硅源至少包括硅粉、正硅酸乙酯、石英砂、白炭黑，硅溶胶中的一种或多种。
3.如权利要求1所述的微波闪烧合成碳化硅的方法，其特征在于步骤(1)中所述的碳源至少包括工业煤、石墨、活性炭、石油焦中的一种或多种。
4.如权利要求1-3任一所述的微波闪烧合成碳化硅的方法，其特征在于碳源和硅源中碳硅摩尔比为0.5～10：1。
5.如权利要求1-3任一所述的微波闪烧合成碳化硅的方法，其特征在于混料方式至少包括球磨法混合或研磨法混合或机械搅拌混合。
6.如权利要求1或4所述的微波闪烧合成碳化硅的方法，其特征在于骤(2)中的成型方式至少包括干压成型、等静压成型、溶胶凝胶成型。
7.如权利要求1或4所述的微波闪烧合成碳化硅的方法，其特征在于步骤(2)中微波烧成时输入功率为3KW～10KW，加热频率为915MHz或2450MHz。
8.如权利要求1或4所述的微波闪烧合成碳化硅的方法，其特征在于最终得到α-SiC。
9.如权利要求8所述的微波闪烧合成碳化硅的方法，其特征在于所制备的α-SiC为典型的六方结构。
10.如权利要求8或9所述的微波闪烧合成碳化硅的方法，其特征在于所制备的α-SiC在制备半导体材料、功能陶瓷、高级耐火材料中的应用。
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