CN118201893A - 制造碳化或石墨化的三维物体的方法 - Google Patents
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Abstract
本发明涉及一种制造碳化或石墨化的3D物体的方法，其目的是特别简单地制造这种3D物体，并且通过这种方法还可以生产出结构上没有缺陷的更复杂的3D物体。实现方法包括：将可碳化或可石墨化的材料与自由流动的有机粘合剂或自由流动的热塑性有机物质混合，制备可塑且尺寸基本稳定的化合物，并将该化合物塑形为3D坯件，然后在预定时间段内以较高温度进行干燥和脱气处理，随后在保护气体的氛围中将3D坯件放入熔炉中进行碳化或石墨化处理，以生成3D物体，其中碳化或石墨化所需的温度以较低的加热梯度接近。
Description
技术领域
本发明涉及一种制造碳化或石墨化的三维(3D)物体的方法。
背景技术
这种碳化或石墨化的三维物体也适用于高温应用，其可以是各种部件，如熔炉内衬、建筑部件或任何所需的空心体、容器或坩埚。
由于不可能通过碳黑或石墨的简单塑形和随后的烧结来生产三维物体，因此一般需要生产一种合适的含碳可塑性化合物。这通常包括将颗粒状的炭黑、焦炭或石墨与适当的粘合剂(如热塑性粘合剂)混合。有用的粘合剂还包括基于煤焦油或石油沥青的沥青，或者其他合成树脂。
然后，这些混合物通过压制形成原始成型件(green molding)，并在约3000℃的炉中碳化或石墨化，而粘合剂分解成挥发性成分。剩下的是碳和粘合剂焦炭，它们是以多孔微结构形式存在的粘合剂残留物。
或者，也可以将原始成型件作为电阻元件放置在电极之间的熔炉中，并通过电流加热。
这种成型件的碳化或石墨化的问题在于，在所需的高温条件下，挥发性物质会或多或少地剧烈放气，从而导致微观结构缺陷，如裂缝或气体夹杂物。
发明内容
本发明的目的是提供一种生产碳化或石墨化的3D物体的方法，这种方法实现起来特别简单，甚至可以生产出没有微观结构缺陷的相对复杂的3D物体。
实现方法包括：制备由可碳化或可石墨化的材料和自由流动的有机粘合剂或自由流动的热塑性有机材料组成的可塑且尺寸基本稳定的化合物，并将该化合物塑形以形成3D坯件，然后在高温下进行干燥和脱气处理，随后在减压或保护气体的作用下，将3D坯件放入熔炉中进行碳化或石墨化，从而生产3D物体，碳化或石墨化所需的温度以较低的加热梯度接近。
有用的可碳化或可石墨化的材料优选是炭黑、石墨粉、天然石墨、纸浆或玉米淀粉，或这些材料中的部分或全部的混合物。
为了影响要制造的3D物体的强度或孔隙率，可以在可碳化或可石墨化的材料中添加竹、棉、麻、剑麻或石墨纤维，并同时保持可塑性。
在第一实施例中，3D坯件的塑形是借助合适的模板手工完成的。
在特定的实施例中，3D坯件是通过在模具中塑形而制成的。
使用的保护气体优选是氩气或氦气。
可替代地，3D坯件在干燥过程之后，可以在稳定温度为170℃的空气中或最高450℃的空气中进行稳定化和均化操作，优先考虑250℃的温度，从而形成3D成型件。
稳定化和均化操作原则上也可以在保护气体(如氩气)下进行。
3D坯件的稳定化和均化也可以在加热熔炉时实现。
在本发明的进一步实施例中，在约1000℃的恒温条件下对3D成型件进行碳化，直至形成不同晶体结构的纯碳，从而形成3D物体。
在本发明的另一种实施例中，3D成型件是在2000℃以上的恒温条件下进行石墨化的。
最后，3D成型件可以在超过2500℃的温度下完全石墨化。
优选地，以每分钟约1℃的加热速度进行石墨化，直至达到目标温度，然后根据3D成型件的大小，进行约30分钟的热处理。
在本发明的一个特定实施例中，可在可塑性化合物中添加金属粉末或硅粉，从而在保护气体作用下，在3D成型件的大于1000℃的高温处理中形成金属碳化物或硅碳化物。
在熔炉中，在大于1200℃的温度下，以氩气为载气供应气态SiO，压力约为30毫巴(mbar)，石墨化的泡沫结构的3D物体还可以转化为由碳化硅(SiC)制成的3D物体。
具体实施方式
下文将根据一个示例性实施方案对本发明进行更详细的解释。
在第一方法步骤中，通过将可碳化或可石墨化的材料与自由流动的有机粘合剂或自由流动的热塑性有机材料混合，制备可塑且尺寸基本稳定的化合物，然后对化合物进行塑形，从而形成3D坯件。然后，在高温下进行干燥和脱气处理，去除3D坯件中的水分和气体夹杂物，从而将3D坯件转化为3D成型件。这样可以避免3D成型件在减压或保护气体(如氩气或氦气)作用下的熔炉中进行后续的碳化或石墨化以生产3D物体时形成裂缝。
所使用的可碳化或可石墨化的有机材料优选是炭黑、石墨粉、天然石墨或淀粉(例如玉米淀粉或马铃薯淀粉或类似材料)，或这些材料的部分或全部混合物。
为了影响碳化或石墨化的3D物体成品的强度或孔隙率，可以在保持可塑性的前提下，向碳化或可石墨化的有机材料中添加竹、棉、麻、剑麻或其他合适的植物纤维或石墨纤维，并且根据需要进一步添加自由流动的粘合剂或自由流动的有机材料，直到达到所需的稠度。
3D坯件的塑形可以通过手工完成(例如借助模板)，也可以在模具中塑形，在这种情况下，应在干燥过程之前将3D坯件从模具中取出。为了便于3D坯件的脱模，可以使用聚四氟乙烯、硅胶或其他具有一定弹性的材料制成的模具。
可替代地，在室温或最高温度为100℃的条件下进行干燥以去除水分后，再进行三维成型。在保护气体或减压条件下，在稳定温度为140℃的空气中或最高450℃的温度下进行后续稳定化和均化操作，优先考虑250℃的温度进行稳定化和均化操作，并且进行脱气，以避免在后续碳化或石墨化过程中形成裂缝。
可以理解的是，在稳定化或均化操作过程中，3D成型件可以保持在合适的模具中。
在加热熔炉的同时，还可以实现3D成型件的稳定化和均化。
为了防止3D成型件在碳化/石墨化过程中被破坏，必须对3D成型件进行稳定处理，否则3D成型件可能会熔化或严重变形。在稳定过程中，原子/分子会发生重新排列，从而使它们在高温过程中得以存在。
在进一步的实施例中，在熔炉中，在约1000℃的恒温条件下，对3D成型件进行碳化，直至形成不同晶体结构的纯碳，从而形成3D物体。
在本发明的另一个实施例中，3D成型件随后在熔炉中在2000℃以上的恒温下进行石墨化，以形成3D物体。
最后，3D成型件可在熔炉中在超过2500℃的温度下完全石墨化，形成3D物体。
应该理解，熔炉内的碳化或石墨化必须在保护气体下进行，以避免3D坯件中的有机成分燃烧。
如果在减压条件下进行碳化或石墨化(原则上是可行的)，则存在这样的风险，即压力差会导致挥发性成分在3D成型件内部和减压之间加速流动，从而形成裂缝。
因此，在熔炉中提供较高的压力是有好处的，这样挥发性成分就会慢慢扩散出来，从而可以安全地避免裂缝和断裂。
优选地，碳化或石墨化以每分钟约1℃的加热速度进行，直到达到目标温度，然后再进行约30分钟的热处理，也可以进行数小时的热处理。
为了实现均匀的碳化或石墨化，建议事先对3D成型件进行脱模。
在本发明的一个特定实施例中，可在可塑化合物中添加金属粉末或硅粉，从而在保护气体作用下，在三维成型件的大于1000℃的高温处理中形成金属碳化物或硅碳化物。
在熔炉中，在大于1200℃的温度下，以氩气为载气供应气态SiO，压力约为30毫巴，石墨化的泡沫结构的3D物体还可以转化为由碳化硅制成的3D物体。
Claims (11)
1.一种制造碳化或石墨化的3D物体的方法，其特征在于，将由炭黑、石墨粉、天然石墨、纸浆或玉米淀粉或这些材料的部分或全部材料的混合物组成的可碳化或可石墨化的材料与自由流动的有机粘合剂或自由流动的热塑性有机材料混合，以形成可塑且尺寸稳定的化合物，并借助特氟龙或硅树脂制成的模具将所述化合物塑形以形成3D坯件，然后将3D坯件从模具中取出，随后在室温或最高100℃的温度下，在预定时间段内进行干燥和脱气处理，然后在140℃至最高450℃的温度下进行稳定化和均化操作，随后在保护气体的氛围下，在熔炉中对3D坯件进行碳化或石墨化，从而生产3D物体，其中碳化或石墨化所需的温度以每分钟1℃的加热速度接近，然后进行热处理。
2.根据权利要求1所述的方法，其特征在于，在可碳化或可石墨化的材料中加入竹、棉、麻、剑麻或石墨纤维，同时保持塑性。
3.根据权利要求1和2所述的方法，其特征在于，3D坯件的塑形是通过手工和/或借助模板进行的。
4.根据权利要求3所述的方法，其特征在于，3D坯件的稳定化和均化是在加热熔炉的同时进行的。
5.根据权利要求1至4中任一项所述的方法，其特征在于，在减压或保护气体的作用下，在1000℃的恒温条件下对3D成型件进行碳化，直至形成不同晶体结构的纯碳，从而形成3D物体。
6.根据权利要求1至5中任一项所述的方法，其特征在于，3D成型件是在减压或保护气体的作用下在熔炉内进行石墨化，以在2000℃以上的恒温条件下形成3D物体。
7.根据权利要求6所述的方法，其特征在于，在减压或保护气体的作用下，3D成型件在熔炉内完全石墨化，以在超过2500℃的温度下形成3D物体。
8.根据权利要求1至7中任一项所述的方法，其特征在于，所用的保护气体为氩气或氦气。
9.根据权利要求7和8所述的方法，其特征在于，3D成型件的石墨化的加热速度约为1℃/分钟，直至达到目标温度，然后进行约30分钟至数小时的热处理。
10.根据权利要求1至9中任一项所述的方法，其特征在于，在可塑的化合物中加入金属粉末或硅粉，从而在保护气体的作用下，在熔炉中，在大于1000℃的温度下对3D坯件进行高温处理，使得生产出包括金属碳化物或硅碳化物的3D成型件。
11.根据权利要求1至10中任一项所述的方法，其特征在于，在大于1200℃的温度下，在30毫巴的压力下，以氩气为载气供应气态SiO，在熔炉中将石墨化的泡沫结构的3D物体转化为由SiC制成的3D物体。
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