CN116462512A - 一种增材制造的高致密纯碳化硅及其制备方法和应用 - Google Patents
一种增材制造的高致密纯碳化硅及其制备方法和应用 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 239000000654 additive Substances 0.000 title claims abstract description 31
- 230000000996 additive effect Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 5
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 3
- 239000003758 nuclear fuel Substances 0.000 claims description 3
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- 229910018540 Si C Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
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- 238000002791 soaking Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
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Abstract
本发明涉及一种增材制造的高致密纯碳化硅及其制备方法和应用，属于碳化硅增材制造技术领域。具体制备方法：首先在获得的薄层碳化硅粉末床的表面建立气流场、厚度方向建立温度梯度场，再将氩气、氢气和含Si与C的前驱气体形成的混合气体沿其表面向厚度方向扩散，当扩散至900～1400℃温度区后由下至上在薄层碳化硅粉末床的孔隙间沉积生长碳化硅，从而致密化了该薄层碳化硅粉末床，最后以该致密化的粉末床为基础重复上述步骤直至制备出三维结构的碳化硅。CVI(化学气相渗透)结合增材制造获得的碳化硅孔隙率的非均匀性可以控制在薄层碳化硅粉末床的厚度尺寸以内，避免了三维碳化硅内部整体存在孔隙梯度分布从而导致局部失效的问题。
Description
技术领域
本发明属于碳化硅增材制造技术领域，涉及一种增材制造的高致密纯碳化硅及其制备方法和应用。
背景技术
碳化硅因其具有高模量值、高热稳定性、高比强度，不易变形且具有较高的导热系数和低的热膨胀系数的特点成为了一种优良的结构材料，目前已被广泛应用于核工业、航空航天、机械制造和微电子工业等领域。但是，由于碳化硅中存在键能很高的Si-C共价键，一方面导致其硬度极高，加工难度大；另一方面导致其熔点高，难以实现致密化烧结。因此，碳化硅成为了典型的难加工材料，极大地限制了其在各领域中的应用。寻找易于制备碳化硅的方法是一个急需解决的问题。
相较于碳化硅的传统制备方式，增材制造的制备方法在无需模具、可成型复杂部件等方面具有巨大优势，从而成为了科研学者的研究热点。目前，主流的碳化硅增材制造技术包括以陶瓷聚合物先驱体为原料的立体光固化工艺和墨水直写工艺。其中，立体光固化工艺是将聚合物制作成线状材料，然后将这些线材通过熔融沉积成型(FDM)打印机的喷嘴加热熔融并挤出，伴随着喷头的运动，在基底面上层层沉积形成设计好的形状，最终制成需要的零部件。但是该工艺在实际操作中存在以下问题：①聚合物热解后残碳量较高；②激光选区烧结成形配合反应烧结后处理工艺残硅量较高；③聚合物浸渍裂解工艺尺寸精度难以控制。这些问题会导致碳化硅的具体应用场合受到限制。而墨水直写工艺是将高黏度的液体或固液混合浆料作为墨水材料存储于料筒中并与喷头相连，然后安装于能够在计算机控制下完成三维运动的三轴CNC平台上，通过机械压力或气动压力推动墨水材料从喷头连续挤出并在基底上预成型，再依据材料特性进行挥发溶剂、热固化、光固化、烧结或浸泡等处理，得到最终的三维成型构件。然而该工艺在实际操作中存在墨水直写或凝胶铸造配合液相烧结工艺温度过高的问题，这也使得制备的碳化硅的应用场景受到约束，同时碳化硅在高温条件下不耐受，难以使用。
因此，为了解决目前碳化硅增材制造技术中存在的诸如碳化硅使用场景受限、高温条件难以使用、纯度不高等问题，有必要开发一种新型的碳化硅的增材制造的方法。
发明内容
有鉴于此，本发明的目的之一在于提供一种增材制造的高致密纯碳化硅的制备方法；本发明的目的之二在于提供一种增材制造的高致密纯碳化硅；本发明的目的之三在于提供一种增材制造的高致密纯碳化硅在核燃料一体化成形制造方面的应用。
为达到上述目的，本发明提供如下技术方案：
1.一种增材制造的高致密纯碳化硅的制备方法，所述制备方法如下：
(1)制备薄层碳化硅粉末床：将碳化硅粉末置于模具中，通过挤压碳化硅粉末得到致密度大于40％、具有孔隙结构的薄层碳化硅粉末床；
(2)建立气流场和温度梯度场：在步骤(1)中所述薄层碳化硅粉末床的表面建立气流场、厚度方向建立温度梯度场；
(3)CVI致密化薄层碳化硅粉末床：将氩气、氢气和前驱气体形成的混合气体沿步骤(1)中所述薄层碳化硅粉末床的表面向厚度方向扩散，所述混合气体扩散至900～1400℃的高温区后由下至上在所述薄层碳化硅粉末床的孔隙间沉积生长碳化硅即可形成致密化薄层碳化硅粉末床；
所述前驱气体包括SiCl4和CH4形成的混合物或CH3SiCl3中的任意一种；
(4)增材制造高致密纯碳化硅：在步骤(3)中所述致密化薄层碳化硅粉末床的表面重复进行步骤(1)～(3)的过程两次以上即可获得三维的高致密纯碳化硅。
优选的，步骤(1)中所述挤压的压力为1～100MPa。
优选的，步骤(2)中所述气流场中气流的方向为从所述薄层碳化硅粉末床的表面流向厚度方向；所述温度梯度场中所述薄层碳化硅粉末床的厚度每增加0.01～0.1mm，温度提高10～100℃。
优选的，步骤(3)中所述氩气、氢气和前驱气体的摩尔比为不低于10:10:1。
优选的，步骤(3)中所述前驱气体的扩散速率与所述碳化硅的生长速率成正相关。
2.所述方法制备的高致密纯碳化硅。
3.所述高致密纯碳化硅在核燃料一体化成形方面的应用。
本发明的有益效果在于：本发明提供了一种增材制造的高致密纯碳化硅。该碳化硅在制备过程中先建立薄层碳化硅粉末床，然后在该粉末床的表面建立气流速度不受约束的气流场、厚度方向建立温度梯度场，再将氩气、氢气和前驱气体(SiCl4和CH4的混合物或CH3SiCl3)形成的混合气体沿该粉末床的表面向厚度方向扩散，当该混合气体扩散至900～1400℃的高温区后由下至上在粉末床的孔隙间沉积生长碳化硅，从而完成了薄层碳化硅粉末床的致密化成形，以该致密化的薄层碳化硅粉末床为基础重新铺放一层(或多层)薄层碳化硅粉末床，重复上述步骤直至完成三维结构的高致密纯碳化硅的制备。本发明实现了高致密度和高纯度的碳化硅的制备，同时利用CVI(化学气相渗透)和增材制造获得的碳化硅孔隙率的非均匀性可以控制在薄层碳化硅粉末床的厚度尺寸以内，避免了最终制备的三维碳化硅内部整体存在孔隙梯度分布从而导致局部失效的问题。该制备方法简单易操作、适合扩大化生产。
本发明的其他优点、目标和特征在某种程度上将在随后的说明书中进行阐述，并且在某种程度上，基于对下文的考察研究对本领域技术人员而言将是显而易见的，或者可以从本发明的实践中得到教导。本发明的目标和其他优点可以通过下面的说明书来实现和获得。
附图说明
为了使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明作优选的详细描述，其中：
图1为本申请中的高致密纯碳化硅的增材制造过程示意图。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。需要说明的是，以下实施例中所提供的图示仅以示意方式说明本发明的基本构想，在不冲突的情况下，以下实施例及实施例中的特征可以相互组合。
实施例1
一种增材制造的高致密纯碳化硅，其具体制备过程如下：
(1)制备薄层碳化硅粉末床：将碳化硅粉末置于异形模具中，以100MPa挤压碳化硅粉末得到致密度为92％、具有孔隙结构的薄层碳化硅粉末床；
(2)建立气流场和温度梯度场：在步骤(1)中薄层碳化硅粉末床的表面建立气流场、厚度方向建立温度梯度场(其中薄层碳化硅粉末床的厚度每增加0.1mm，温度提高100℃)；
(3)CVI致密化薄层碳化硅粉末床：将氩气、氢气和CH3SiCl3按10:10:1的摩尔比混合均匀，然后沿步骤(1)中薄层碳化硅粉末床的表面向厚度方向扩散，当混合气体扩散至900～1400℃的高温区后由下至上在该薄层碳化硅粉末床的孔隙间沉积生长碳化硅即可形成致密化薄层碳化硅粉末床；
(4)增材制造高致密纯碳化硅：在步骤(3)中致密化薄层碳化硅粉末床的表面重复进行步骤(1)～(3)的过程两次即可获得三维的高致密纯碳化硅。
实施例2
一种增材制造的高致密纯碳化硅，其具体制备过程如下：
(1)制备薄层碳化硅粉末床：将碳化硅粉末置于异形模具中，以10MPa挤压碳化硅粉末得到致密度为42％、具有孔隙结构的薄层碳化硅粉末床；
(2)建立气流场和温度梯度场：在步骤(1)中薄层碳化硅粉末床的表面建立气流场、厚度方向建立温度梯度场(其中薄层碳化硅粉末床的厚度每增加0.01mm，温度提高10℃)；
(3)CVI致密化薄层碳化硅粉末床：将氩气、氢气和由SiCl4和CH4形成的混合物按10:10:1的摩尔比混合均匀，然后沿步骤(1)中薄层碳化硅粉末床的表面向厚度方向扩散，当混合气体扩散至900～1400℃的高温区后由下至上在该薄层碳化硅粉末床的孔隙间沉积生长碳化硅即可形成致密化薄层碳化硅粉末床；
(4)增材制造高致密纯碳化硅：在步骤(3)中致密化薄层碳化硅粉末床的表面重复进行步骤(1)～(3)的过程三次即可获得三维的高致密纯碳化硅。
图1为本申请中的高致密纯碳化硅的增材制造过程示意图。从图1中可以看出制备该高致密纯碳化硅的关键过程为化学气相浸渗和增材制造。化学气相浸渗具有生成碳化硅晶体种类和残留物(碳、硅其它前驱体以及反应中间产物)精确可控的优势，通过控制化学气相浸渗的工艺参数，可以制备出高纯度的碳化硅。同时结合增材制造，每沉积生长一层碳化硅粉末床，结合一次致密化过程，从而保证了每生长的碳化硅粉末床都是致密化的，最终实现了整体结构的致密化。
综上所述，本发明提供了一种增材制造的高致密纯碳化硅。制备该高致密纯碳化硅的关键过程为化学气相浸渗和增材制造。其中，化学气相浸渗法可以确保制备的碳化硅具有高纯度，结合增材制造可以使高纯度的碳化硅进一步致密化。其制备方法简单、易操作、适合扩大化生产。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。
Claims (7)
1.一种增材制造的高致密纯碳化硅的制备方法，其特征在于：所述制备方法如下：
(1)制备薄层碳化硅粉末床：将碳化硅粉末置于模具中，通过挤压碳化硅粉末得到致密度大于40％、具有孔隙结构的薄层碳化硅粉末床；
(2)建立气流场和温度梯度场：在步骤(1)中所述薄层碳化硅粉末床的表面建立气流场、厚度方向建立温度梯度场；
(3)CVI致密化薄层碳化硅粉末床：将氩气、氢气和前驱气体形成的混合气体沿步骤(1)中所述薄层碳化硅粉末床的表面向厚度方向扩散，所述混合气体扩散至900～1400℃的高温区后由下至上在所述薄层碳化硅粉末床的孔隙间沉积生长碳化硅即可形成致密化薄层碳化硅粉末床；
所述前驱气体包括SiCl4和CH4形成的混合物或CH3SiCl3中的任意一种；
(4)增材制造高致密纯碳化硅：在步骤(3)中所述致密化薄层碳化硅粉末床的表面重复进行步骤(1)～(3)的过程两次以上即可获得三维的高致密纯碳化硅。
2.根据权利要求1所述的制备方法，其特征在于：步骤(1)中所述挤压的压力为1～100MPa。
3.根据权利要求1所述的制备方法，其特征在于：步骤(2)中所述气流场中气流的方向为从所述薄层碳化硅粉末床的表面流向厚度方向；所述温度梯度场中所述薄层碳化硅粉末床的厚度每增加0.01～0.1mm，温度提高10～100℃。
4.根据权利要求1所述的制备方法，其特征在于：步骤(3)中所述氩气、氢气和前驱气体的摩尔比为不低于10:10:1。
5.根据权利要求1所述的制备方法，其特征在于：步骤(3)中所述前驱气体的扩散速率与所述碳化硅的生长速率成正相关。
6.根据权利要求1～5任一项所述的方法制备的高致密纯碳化硅。
7.权利要求6所述的高致密纯碳化硅在核燃料一体化成形方面的应用。
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