CN111699164A - 含有金属碳化物颗粒的含水悬浮液 - Google Patents

含有金属碳化物颗粒的含水悬浮液 Download PDF

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CN111699164A
CN111699164A CN201980011620.6A CN201980011620A CN111699164A CN 111699164 A CN111699164 A CN 111699164A CN 201980011620 A CN201980011620 A CN 201980011620A CN 111699164 A CN111699164 A CN 111699164A
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hours
suspension
substrate
coating
aqueous suspension
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斯坦尼斯洛斯·施万克
斯蒂芬·穆勒
埃尔克·迈斯纳
鲍里斯·埃佩尔鲍姆
克里斯蒂安·赖曼
约亨·弗里德里希
卢卡斯·贝克尔
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Abstract

本发明涉及包含30重量％至95重量％的金属碳化物颗粒和分散剂的含水悬浮液，并涉及使用所述含水悬浮液涂覆基材的方法。本发明还涉及能够通过根据本发明的方法制备的经涂覆的基材及其用途。

Description

含有金属碳化物颗粒的含水悬浮液
本发明涉及包含金属碳化物颗粒和分散剂的含水悬浮液，并涉及使用这些含水悬浮液涂覆基材的方法。本发明还涉及可通过根据本发明的方法制备的经涂覆的基材及其用途。
高熔点金属碳化物，例如钛、锆、铪、铌、钽、铬、钼、钨和硅的碳化物具有高的机械稳定性、化学稳定性和热稳定性。因此，碳化材料以固体陶瓷体或涂层的形式广泛使用。例如，在高温和/或化学侵蚀性环境下的材料制备中，在切削工具或发动机喷嘴的制备中，以及在晶体生长中使用碳化物材料。
但是，它们的机械硬度使金属碳化物难以加工。这意味着具有难度相对复杂的几何形状的固体成形体只能困难且成本昂贵地由这些材料制备。因此，结构部件大多只涂覆有金属碳化物。
常用的涂层工艺是CVD(化学气相沉积)和PVD(物理气相沉积)工艺。然而，通过这些工艺可获得的涂层通常最多仅几微米厚，这由于长期稳定性差而不足以用于某些应用，例如不足以用于制备碳化硅或氮化铝晶体。
现有技术还包括通过湿法陶瓷工艺制备的金属碳化物涂层的描述，其中通过刷涂、喷涂或浸涂，然后进行烧结工艺，将金属碳化物颗粒的有机悬浮液施加到待涂覆的部件上。
US 2013/0061800 A1描述了一种高度热稳定的元件，其包含含有各向同性石墨的石墨基材。高度热稳定的元件还包含含有碳化物例如碳化钽的碳化物涂层。另外，描述了用于制备所述元件的方法，其中碳化物颗粒由悬浮液沉积在基材上。这是使用有机溶剂作为液相的悬浮液来完成的。
D.Nakamura、T.Kimura、T.Narita、A.Suzumura、T.Kimoto和K.Nakshima在Journalof Crystal Growth，478卷，2017的163页至173页以及D.Nakamura、K.Shigetoh和A.Suzumura在the Journal of the European Ceramic Society，37卷，2017的1175页至1185页也描述了用碳化钽涂覆石墨的湿法陶瓷工艺。在公开的方法中，碳化钽是由基于有机溶剂的悬浮液沉积出来的。
现有技术中已知的湿法陶瓷工艺允许制备相对较厚的层，其中该层在某些情况下为几百微米厚。与通过CVD或PVD工艺制备的层相反，通过湿法陶瓷工艺制备的层具有各向同性的结构，具有随机的颗粒取向，从而降低了对裂纹的敏感性，并增强了破坏基材的物质的扩散途径。
然而，基于有机溶剂的悬浮液具有重要的缺点。除了由有机溶剂的毒性引起的生态和健康方面的考虑之外，使用此类悬浮液还带来高度易燃喷雾的安全性问题。此外，必须通过热解除去有机溶剂。这导致异物不必要地引入涂层中。此外，对于已知的悬浮液，特别是在喷涂工艺中，不可能对悬浮液进行受控施加，因为在所述工艺中由于溶剂的蒸发悬浮液的性质可能会发生波动，这意味着随着时间的流逝，将不再可能获得均匀的层。
另外期望能够影响碳化物涂层中的开孔与闭孔的比率，这对于已知的基于有机溶剂的悬浮液仅在有限的程度上是可能的。另一个理想的目的是获得在基材表面具有更大渗透深度的涂层的能力。
基于此，本发明的目的是提供不存在任何生态、健康和安全问题的悬浮液。还可以由非常纯且不需要热解步骤的悬浮液制备涂层。使用所提供的悬浮液，还应该能够随时间沉积非常均匀的层，并控制从悬浮液沉积的涂层中的开孔和闭孔之间的比率。另外，应当增加从提供的悬浮液沉积的涂层距离待涂覆的基材表面的渗透深度。此外，涂层应具有低的气体渗透性、高的抗热震性，并且对于化学侵蚀性气氛稳定。
通过使用包含有机溶剂作为液相的悬浮液而引起的生态、健康和安全问题可以通过使用水作为液相来消除。
但是，由于各种原因，到目前为止，尚不认为水是金属碳化物悬浮液的液相。首先，金属碳化物具有很高的密度(碳化钨15.6g/cm3，碳化钽13.9g/cm3)，因此很快发生偏析。为了沉积具有高均匀性的层，至关重要的是将金属碳化物颗粒悬浮在悬浮液中。
此外，在含水悬浮液中必需具有高固体含量意味着必须预期金属碳化物颗粒的团聚，这会导致开裂并降低由这种悬浮液沉积的涂层的生坯密度。另一方面，有机溶剂可通过其官能团提供至少在一定程度上抑制团聚的选项。
本发明的目的是克服水作为液相时发生的上述问题。
该目的通过具有权利要求1的特征的含水悬浮液来实现，该悬浮液具有以下所列的技术特征。
含水悬浮液包含
至少一种金属碳化物颗粒和
至少一种分散剂，
其中至少一种金属碳化物颗粒的比例为基于悬浮液总重量的30重量％至95重量％。
在权利要求2至4中说明根据本发明的悬浮液的有利实施方案。
如权利要求5所述，本发明还涉及使用本发明的含水悬浮液涂覆基材的方法，该方法包括以下步骤：
i)提供基材；
ii)提供根据本发明的含水悬浮液；
iii)将步骤ii)中的悬浮液施加到步骤i)中的基材表面上；
iv)干燥所施加的悬浮液，在基材表面上形成涂层。
在权利要求6至11中说明了该方法的有利实施方案。
如权利要求12和13所述，本发明还涉及能够通过根据本发明的方法制备的基材，其中权利要求14和15说明了所述基材的用途。
术语的定义
在本发明的上下文中的“含水悬浮液”中，水被用作液相。在所述相中可以存在最多2重量％，优选最多1重量％的其他溶剂。但是，特别优选“含水悬浮液”的液相仅为水。
根据本发明的“平均粒径”应理解为是指d50值，即50％的颗粒具有小于该值的粒径而其他50％的颗粒具有大于该值的粒径。优选通过激光散射直接在悬浮液上确定“平均粒径”。团聚物的大小优选通过激光散射直接在悬浮液上确定。
金属碳化物颗粒或由所述颗粒形成的涂层的“纯度”应理解为是指关于各个元素杂质的化学纯度。纯度优选通过GDMS(辉光放电质谱法)确定。
在本发明的上下文中，涂层的“生坯密度”理解为是指相对于烧结金属碳化物层的理论密度所制备的层的密度。
在本发明的上下文中，类金属硅的碳化物被视为金属碳化物。
所述量
除了水作为液相之外，根据本发明的含水悬浮液还包含至少一种金属碳化物颗粒，至少一种分散剂和任选的添加剂。所述量分别基于悬浮液的总重量，并且所存在的组分的总重量合计为100重量％。
含水悬浮液
根据本发明的含水悬浮液包含至少一种金属碳化物颗粒和至少一种分散剂，其中基于悬浮液的总重量，至少一种金属碳化物颗粒的比例为30重量％至95重量％。金属碳化物颗粒的比例优选通过从悬浮液中除去挥发性成分来确定，这优选通过将悬浮液加热至高于水的蒸发温度的温度来完成。金属碳化物颗粒的比例可以由称量的量确定。
下文指出了根据本发明的含水悬浮液的优选实施方案。
在本发明的一个优选的实施方案中，至少一种金属碳化物颗粒选自钛、锆、铪、钒、铌、钽、铬、钼、钨、硅及其混合物的碳化物，其中优选碳化钽。
本文中优选至少一种金属碳化物颗粒的平均粒径为0.05μm至25μm，更优选为0.5μm至5μm，特别优选为1μm至2μm。
更优选至少一种金属碳化物颗粒的各种元素杂质的含量为＜300ppm，优选＜10ppm，更优选小于1ppm。如果金属碳化物颗粒不能以足够的纯度商购获得，则可以通过本领域技术人员已知的方法将其纯化，例如湿法化学纯化。而且，由含水悬浮液沉积的涂层的纯度不一定对应于所使用的金属碳化物颗粒的纯度。通过下面描述的根据本发明的方法可以除去杂质。
特别优选至少一种金属碳化物颗粒的平均粒径为0.05μm至25μm，更优选0.5μm至5μm，非常特别优选1μm至2μm，并且各种元素杂质的含量为<300ppm，优选<10ppm，更优选小于1ppm。
优选的金属碳化物是碳化钽，其特别优选立方相的相分数为70％至100％。
在另一个优选的实施方案中，分散剂可能选自聚丙烯酸、四丁基氢氧化铵及其混合物，所述聚丙烯酸的数均分子量优选为3000g/mol至10000g/mol，更优选4000g/mol至6000g/mol。
在本发明的另一个优选实施方案中，其包含至少一种添加剂，所述添加剂优选地选自碱、特别是氢氧化钠溶液，消泡剂、特别是脂肪醇聚亚烷基二醇醚，烧结助剂、特别是钴或硅，和其混合物。本文特别优选的添加剂是消泡剂。后者的使用抑制了悬浮液中气泡的形成，从而减少了开裂。
在本发明的另一个优选实施方案中，基于悬浮液的总重量，金属碳化物颗粒的比例可以为40重量％至90重量％，优选为60重量％至85重量％。
在本发明的又一个优选实施方案中，基于悬浮液的总重量，分散剂的比例可以为0.05重量％至5重量％，优选为0.1重量％至2重量％。
在本发明的另一个优选实施方案中，基于悬浮液的总重量，添加剂在悬浮液中的比例为0重量％至10重量％，优选0.5重量％至5重量％。
在本发明的又一个优选实施方案中，基于悬浮液的总重量，金属碳化物颗粒的比例为40重量％至90重量％，优选为60重量％至85重量％，分散剂的比例为0.05重量％至5重量％，优选为0.1重量％至2重量％，并且添加剂在悬浮液中的比例为0重量％至10重量％，优选为0.5重量％至5重量％。
在本发明的另一个优选实施方案中，悬浮液的pH可能为5至10，优选为7至8。当使用聚丙烯酸作为分散剂时，pH优选为7至8。
在另一个优选的实施方案中，含水悬浮液除水、金属碳化物颗粒、分散剂和上述添加剂外不包含其他成分。
在本发明的另一个优选实施方案中，含水悬浮液完全不含有机溶剂。
方法
根据本发明的涂覆基材的方法包括以下步骤：
i)提供基材；
ii)提供本发明的含水悬浮液
iii)将步骤ii)中的悬浮液施加到步骤i)中的基材表面上；
iv)干燥所施加的悬浮液，在基材表面上形成涂层。
下文指出了本发明方法的优选实施方案。
在根据本发明的方法的优选实施方案中，基材选自石墨、具有经调节的热膨胀系数的材料，优选经调节的热膨胀系数为6.5×10-6K-1至7.5×10-6K-1的石墨及其混合物。
在根据本发明的方法的另一个优选实施方案中，该方法可能包括以下另外的步骤：
v)在步骤iii)之前对步骤i)中提供的基材进行预处理，其中优选通过选自表面机械粗糙化、表面热预处理、表面化学处理及其组合的措施进行预处理，随后进行清洁，特别是通过超声处理；
vi)烧结步骤iv)后获得的涂层。
为了获得涂层在基材上的良好黏附性，特别有利的是首先机械地使基材变粗糙，然后通过超声处理通过适当的清洁步骤产生亲水性表面。特别是在石墨基材的情况下，必须注意确保消除或至少减少表面上的松散颗粒的数量。
在另一个优选的实施方案中，通过刷涂、浸涂或喷涂来施加步骤iii)中的悬浮液。
当通过喷涂施加时，基材优选放置在可旋转转盘的中央，并通过特殊的支架固定在适当的位置。转盘的倾斜角和喷枪的喷射角还根据待涂覆的基材的几何形状通过专门指定的支架进行调整。然后，在明确定义的喷雾参数(包括雾化器气压、通过针头提升装置对物料供应的节流以及从喷嘴开口到基材表面的距离)下用含水悬浮液对基材进行涂覆。在喷涂过程中，转盘的旋转速度由后续涂层的所需层厚度决定。
在本发明的另一个优选实施方案中，步骤iv)在100℃至600℃，优选120℃至550℃，更优选145℃至455℃的温度下进行，其中优选在5小时至40小时内，更优选在20小时至30小时内进行步骤iv)。
为了获得无开裂的层，已证明有利的是在多个温度步骤中对步骤iv)中获得的涂层进行退火。为了防止过快干燥和随后的开裂，特别优选包含保持阶段。具体的保持阶段由所用分散剂的蒸发行为决定。当使用钴作为烧结助剂时，有利的是在惰性气体气氛下进行干燥过程。
在优选的干燥过程iv)中，温度范围和时间间隔可以如下：
(1)140℃至160℃持续2.5小时至3.5小时；然后
(2)180℃至220℃持续1.5小时至2.5小时；然后
(3)在(2)的温度下保持2小时；然后
(4)200℃至250℃持续1.5小时至2.5小时；然后
(5)310℃至350℃持续4.5小时至5.5小时；然后
(6)330℃至350℃持续1.5小时至2.5小时；然后
(7)在(6)的温度下保持2小时；然后
(8)380℃至420℃持续3.5小时至4.5小时；然后
(9)430℃至470℃持续1.5小时至2.5小时。
在本发明的另一个优选实施方案中，步骤vi)(＝烧结)在2000℃至2600℃，优选2100℃至2500℃，更优选2200℃至2300℃的温度下进行。特别优选在1小时至10小时内，更优选在3小时至5小时内进行步骤vi)。还优选在500托至900托，优选600托至800托，更优选680托至720托的压力下进行步骤vi)。
在本发明的另一个优选实施方案中，步骤vi)是在惰性气体下进行的，惰性气体特别优选地选自氦、氩、氮及其混合物。
添加烧结助剂例如钴或硅会提高烧结过程中的流动性能，并增加可达到的涂层端部密度。
在本发明的另一个优选实施方案中，在步骤v)之前的涂层的生坯密度为至少50％，优选为至少60％。
在另一个优选的实施方案中，步骤iv)或vi)之后的涂层可能具有小于300ppm，优选小于1ppm的各种元素杂质含量。
在另一个优选的实施方案中，步骤iv)或vi)之后的涂层的开孔孔隙率小于5％，优选小于1％。这优选通过Hg孔隙率法确定。
在本发明的另一个优选实施方案中，步骤iv)或vi)之后的涂层厚度为20μm至500μm，优选为50μm至400μm，更优选为100μm至300μm。
在另一个优选的实施方案中，在步骤iii)之前的含水悬浮液的pH可能为5至10，优选为7至8，特别是对于聚丙烯酸作为分散剂而言。
经涂覆的基材
本发明进一步涉及能够通过根据本发明的方法制备的经涂覆的基材。
在另一个优选的实施方案中，涂层的厚度为20μm至500μm，优选为50μm至400μm，更优选为100μm至300μm。
在另一个优选的实施方案中，步骤iv)或vi)之后的涂层的杂质含量可能小于300ppm，优选小于1ppm。
在另一个优选的实施方案中，步骤iv)或vi)之后的涂层的开孔孔隙率小于5％，优选小于1％。
用途
根据本发明的经涂覆的基材用作碳化物材料。
本文优选在晶体生长的应用中使用，特别是用于PVT(物理气相)工艺、外延工艺和坩埚的应用中。
参考以下实施例更详细地阐明了本发明的目的，而不旨在将其限制于此处所示的具体实施方案。
含水悬浮液的制备1
使用分散搅拌器制备碳化钽含水悬浮液。这是通过依次添加碳化钽粉末(70重量％，总杂质含量：300ppm，H.C.Starck)、聚丙烯酸(0.5重量％，Mw5000g/mol，PolyscienceEurope GmbH)、烧结助剂(0.7重量％的硅，H.C.Starck)、消泡剂(2滴Contraspum、Zschimmer和Schwarz)和蒸馏水(28.8重量％)来完成的。在添加每种成分之间，用搅拌器将悬浮液以每分钟4000转的速度加工15分钟，以确保金属碳化物粉末、分散剂和所用添加剂均匀分散在悬浮液中。用氢氧化钠溶液将悬浮液的pH调节至pH 8。碳化钽的比例为含水悬浮液总重量的70重量％。
含水悬浮液的制备2
使用分散搅拌器制备碳化钽含水悬浮液。这是通过依次添加碳化钽粉末(70重量％，总杂质含量：300ppm，H.C.Starck)、四丁基氢氧化铵(0.5重量％，Sigma Aldrich)、烧结助剂(0.7重量％的硅，H.C.Starck)、消泡剂(2滴Contraspum、Zschimmer和Schwarz)和蒸馏水(28.8重量％)来完成的。在添加每种成分之间，用搅拌器将悬浮液以每分钟4000转的速度加工15分钟，以确保金属碳化物粉末、分散剂和所用添加剂均匀分散在悬浮液中。悬浮液的pH为7。碳化钽的比例为含水悬浮液总重量的70重量％。
悬浮液1和2用于涂覆石墨基材。
借助于喷枪在具有可旋转和可倾斜转盘的涂覆台上进行涂覆。喷枪使用2巴的压缩空气操作，并安装在一个支架上，该支架可以改变与样品的角度和距离。为了涂覆石墨基材(图1举例说明了一个石墨圆柱体)，选择了19cm的距离和90°的喷射角。考虑到圆柱的几何形状，按照图1所示的装配对石墨圆柱的内部进行了涂覆。为此，将圆柱体固定在转台上并倾斜50°的角度。枪口位于21cm的距离处，水平倾斜角度为70°(图1)。在工作台同时旋转的情况下，通过垂直于气缸壁的向上和向下移动来手动涂覆外部。
为了确定相应层的烧结密度，在实际的烧结步骤之后，确定由此获得的层的质量、厚度和面积，由层的厚度和面积、体积和质量以及相关的量计算烧结密度，其与TaC的最大理论密度相关(14.3g/cm3)。悬浮液1的涂层烧结密度为54％，悬浮液2的涂层烧结密度为56％。
通过对经涂覆和经烧结的基材的横截面进行分析，两种情况下的层厚可通过扫描电子显微镜和入射光显微镜确定，其均为100μm。

Claims (15)

1.一种含水悬浮液，其包含至少一种金属碳化物颗粒和至少一种分散剂，其中基于所述悬浮液的总重量，所述至少一种金属碳化物颗粒的比例为30重量％至95重量％。
2.根据权利要求1所述的含水悬浮液，其特征在于
至少一种金属碳化物颗粒选自钛、锆、铪、钒、铌、钽、铬、钼、钨、硅的碳化物及其混合物，其中优选碳化钽；和
其中至少一种金属碳化物颗粒的平均粒径优选为0.05μm至25μm，更优选为0.5μm至5μm，特别优选为1μm至2μm，和/或
至少一种金属碳化物颗粒的各种元素杂质的含量优选为<300ppm，更优选<10ppm，特别优选<1ppm；和/或
分散剂选自聚丙烯酸、四丁基氢氧化铵及其混合物，所述聚丙烯酸的数均分子量优选为3000g/mol至10000g/mol，更优选4000g/mol至6000g/mol。
3.根据权利要求1或2所述的含水悬浮液，其特征在于
所述含水悬浮液包含至少一种添加剂，所述添加剂选自碱、特别是氢氧化钠溶液，消泡剂、特别是脂肪醇聚亚烷基二醇醚，烧结助剂、特别是钴或硅，及其混合物。
4.根据前述权利要求中任一项所述的含水悬浮液，其特征在于
基于悬浮液的总重量，金属碳化物颗粒的比例为40重量％至90重量％，优选60重量％至85重量％；和/或
基于悬浮液的总重量，分散剂的比例为0.05重量％至5重量％，优选0.1重量％至2重量％；和/或
基于悬浮液的总重量，至少一种添加剂的比例为0重量％至10重量％，优选0.5重量％至5重量％。
5.一种用于涂覆基材的方法，其包括以下步骤：
i)提供基材；
ii)提供权利要求1至4中任一项所述的含水悬浮液；
iii)将步骤ii)中的悬浮液施加到步骤i)中的基材的表面上；
iv)干燥所施加的悬浮液，在所述基材的表面上形成涂层。
6.根据权利要求5所述的方法，其特征在于
基材选自石墨、具有经调节的热膨胀系数的材料，优选经调节的热膨胀系数为6.5×10-6K-1至7.5×10-6K-1的石墨及其混合物。
7.根据权利要求5或6所述的方法，其特征在于
所述方法包括以下其他步骤：
v)在步骤iii)之前对步骤i)中提供的基材进行预处理，其中优选通过选自表面机械粗糙化、表面热预处理、表面化学处理及其组合的措施进行预处理，随后进行清洁，特别是通过超声处理；
vi)烧结步骤iv)后获得的涂层。
8.根据权利要求5至7中任一项所述的方法，其特征在于
通过刷涂、浸涂或喷涂来施加步骤iii)中的悬浮液。
9.根据权利要求5至8中任一项所述的方法，其特征在于
步骤iv)在100℃至600℃，优选120℃至550℃，更优选145℃至455℃的温度下进行，优选在5小时至40小时内，更优选在20小时至30小时内进行步骤iv)，干燥过程iv)特别优选其中温度分阶段升高，最优选以下温度范围和时间间隔：
(1)140℃至160℃持续2.5小时至3.5小时；然后
(2)180℃至220℃持续1.5小时至2.5小时；然后
(3)在(2)的温度下保持2小时；然后
(4)200℃至250℃持续1.5小时至2.5小时；然后
(5)310℃至350℃持续4.5小时至5.5小时；然后
(6)330℃至350℃持续1.5小时至2.5小时；然后
(7)在(6)的温度下保持2小时；然后
(8)380℃至420℃持续3.5小时至4.5小时；然后
(9)430℃至470℃持续1.5小时至2.5小时；
和/或
步骤vi)在2000℃至2600℃，优选2100℃至2500℃，更优选2200℃至2300℃的温度下进行，优选在1小时至10小时内，更优选在3小时至5小时内进行步骤vi)；和/或
在500托至900托，优选600托至800托，更优选680托至720托的压力下进行步骤vi)；和/或
在惰性气体下进行步骤vi)，惰性气体优选地选自氦、氩、氮及其混合物。
10.根据权利要求5至9中任一项所述的方法，其特征在于
在步骤iv)之后和/或在步骤vi)之前，涂层的生坯密度为至少50％，优选至少60％；和/或
步骤iv)或vi)之后的涂层的杂质含量小于300ppm，优选小于1ppm；和/或
步骤iv)或vi)之后的涂层的开孔孔隙率小于5％，优选小于1％。
11.根据权利要求5至10中任一项所述的方法，其特征在于
步骤iv)或vi)之后的涂层厚度为20μm至500μm，优选为50μm至400μm，更优选为100μm至300μm；和/或
在步骤iii)之前的含水悬浮液的pH为5至10，优选为7至8，特别是对于聚丙烯酸作为分散剂而言。
12.一种经涂覆的基材，其能够通过权利要求5至11中任一项所述的方法制备。
13.根据权利要求12所述的经涂覆的基材，其特征在于
涂层的厚度为20μm至500μm，优选为50μm至400μm，更优选为100μm至300μm。
14.根据权利要求12或13中任一项所述的经涂覆的基材作为碳化物材料的用途。
15.根据权利要求14所述的用途，其用于晶体生长的应用中，特别是用于物理气相工艺、外延工艺的应用中和用于坩埚的应用。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106699228A (zh) * 2016-12-19 2017-05-24 北京世纪金光半导体有限公司 一种低成本碳化钽涂层的制备方法
WO2017130134A1 (en) * 2016-01-27 2017-08-03 Consiglio Nazionale Delle Ricerche Composite material based on c/sic fibers with ultra-refractory, high tenacity and ablation resistant matrix
CN107500781A (zh) * 2017-09-28 2017-12-22 上海应用技术大学 一种多孔陶瓷的制备方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19749082A1 (de) * 1997-11-06 1999-05-12 Bayer Ag Nanoskalige anorganische Pigmente enthaltende Ink-Jet-Tinten
JP2001206771A (ja) * 2000-01-21 2001-07-31 Asahi Glass Co Ltd ＳｉＣ治具およびその製造法
JP2008501612A (ja) * 2004-06-08 2008-01-24 トライアンフ，オペレーティング アズ ア ジョイント ヴェンチャー バイ ザ ガバナーズ オブ ザ ユニバーシティ オブ アルバータ，ザ ユニバーシティ オブ ブリティッシュ コロンビア，カールトン 複合セラミック対象物の形成方法
US20060110626A1 (en) * 2004-11-24 2006-05-25 Heraeus, Inc. Carbon containing sputter target alloy compositions
DE102005040157A1 (de) * 2005-08-25 2007-03-01 Degussa Ag Paste aus nanoskaligem Pulver und Dispergiermittel
KR101190561B1 (ko) * 2008-04-04 2012-10-16 토토 가부시키가이샤 복합 재료 및 그의 제조 방법
US8535600B2 (en) * 2009-03-23 2013-09-17 Kabushiki Kaisha Toyota Chuo Kenkyusho High temperature-resistant article, method for producing the same, and high temperature-resistant adhesive
FR2954766B1 (fr) * 2009-12-24 2015-04-24 Saint Gobain Ct Recherches Poudre de granules de ceramique
JP5267709B2 (ja) 2011-09-14 2013-08-21 株式会社豊田中央研究所 高耐熱部材、その製造方法、黒鉛ルツボおよび単結晶インゴットの製造方法
FR2991981A1 (fr) * 2012-06-15 2013-12-20 Saint Gobain Ct Recherches Produit en carbure de silicium pour blindage
CN105175005B (zh) * 2015-10-15 2017-08-29 山东金德新材料有限公司 一种高强均孔碳化硅陶瓷膜的制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017130134A1 (en) * 2016-01-27 2017-08-03 Consiglio Nazionale Delle Ricerche Composite material based on c/sic fibers with ultra-refractory, high tenacity and ablation resistant matrix
CN106699228A (zh) * 2016-12-19 2017-05-24 北京世纪金光半导体有限公司 一种低成本碳化钽涂层的制备方法
CN107500781A (zh) * 2017-09-28 2017-12-22 上海应用技术大学 一种多孔陶瓷的制备方法

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