CN112830786A - 一种碳化硅薄壁结构件的制备方法 - Google Patents
一种碳化硅薄壁结构件的制备方法 Download PDFInfo
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Abstract
本发明公开了一种碳化硅薄壁结构件的制备方法，包括以下步骤：S1、利用石墨基材制作模具；S2、采用化学气相沉积法在石墨基材表面生长碳化硅；S3、从工件的边缘处切割碳化硅包裹部分使内部的石墨基材重新裸露出来；S4、将工件中的石墨基材完全与氧气进行反应，获得固体碳化硅工件。本发明具有碳化硅薄壁结构件具有较高的纯度，有利于避免高温、污染、氧化、腐蚀等问题，有助于提高设备工艺能力和稳定性的优点。
Description
技术领域
本发明涉及半导体装备内部涂层的制备方法，尤其涉及一种碳化硅薄壁结构件的制备方法。
背景技术
目前，在半导体装备领域中，设备反应腔内部由于存在各种腐蚀性化学气氛、高温、电离、颗粒沉积等环境，为了提高设备工艺能力和工艺稳定性，214LD石英件、反应式烧结碳化硅陶瓷及碳化硅涂层石墨是通常应用于设备反应腔内部的选择材料。由于一些设备反应腔体内部温度需要达到甚至超过1300℃，传统的214LD半导体级别石英件会在高温下发生软化，达不到使用要求；反应式烧结碳化硅陶瓷是一种采用碳化硅粉末和其他粘结剂等添加剂材料混合烧结而成，材料的金属杂质含量难以控制，容易对高精度的半导体器件产生污染，导致良率出现问题；碳化硅涂层石墨纯度高，耐高温腐蚀性能好，但在升温、降温的冲击之下，涂层容易出现脱落，导致设备工艺不稳定。
发明内容
本发明要解决的技术问题是克服现有技术的不足，提供一种结构件具有较高的纯度，有利于避免高温、污染、氧化、腐蚀等问题，有助于提高设备工艺能力和稳定性的碳化硅薄壁结构件的制备方法。
为解决上述技术问题，本发明采用以下技术方案：
一种碳化硅薄壁结构件的制备方法，包括以下步骤：
S1、利用石墨基材制作模具；
S2、采用化学气相沉积法在石墨基材表面生长碳化硅；
S3、从工件的边缘处切割碳化硅包裹部分使内部的石墨基材重新裸露出来；
S4、将工件中的石墨基材完全与氧气进行反应，获得固体碳化硅工件。
作为上述技术方案的进一步改进：S2的详细步骤为：
S2.1、将石墨基材放入化学气相沉积设备内，并将化学气相沉积设备抽真空及置换气体；
S2.2、通入氮气，进行预热升温至600～800℃，升温速率1～15℃/min；
S2.3、通入氮气和氢气，继续升温至1400～1600℃，升温速率1～10℃/min；
S2.4、待温场稳定之后，开始通入原料气体、氢气和氩气，以10～200μm/h速率生进行生长。
作为上述技术方案的进一步改进：S2的详细步骤还包括：
S2.5、待碳化硅厚度生长200～500μm时，降温，将工件旋转和/或倒置；
S2.6、重复步骤S2.1至2.5，直到碳化硅总生长厚度达到目标要求。
作为上述技术方案的进一步改进：步骤S2.4中原料气体为三氯甲基硅烷。
作为上述技术方案的进一步改进：步骤S4中，将工件放入高温氧化炉中，升温至900～1200℃，通入氧气，使石墨基材在高温下与氧气进行反应，生成二氧化碳排出，待石墨基材完全反应后获得固体碳化硅工件。
作为上述技术方案的进一步改进：碳化硅薄壁结构件的制备方法还包括步骤：S5、根据目标尺寸和表面形貌要求，对固体碳化硅工件进行抛光、打磨和二次尺寸调整。
作为上述技术方案的进一步改进：碳化硅薄壁结构件的制备方法还包括步骤：还包括步骤：S6、采用10％浓度的氢氟酸进行清洗，然后利用超声波进行去离子水洗，获得成品。
碳化硅薄壁结构件的制备方法步骤S1中，石墨基材的厚度为2-50㎜，表面光洁度在500-1000nm，加工成模具后进行纯化处理。
与现有技术相比，本发明的优点在于：本发明公开的碳化硅薄壁结构件的制备方法，采用全固态沉积碳化硅材料制作结构件，纯度最高可达99.9999％，Fe、Al、Cu、Zn等金属杂质可降至ppb(part per billion，十亿分比浓度)级别，结合碳化硅本身的材料特性，可有效地避免高温、污染、氧化、腐蚀、材料强度等问题，能广泛地应用于SiC氧化炉设备、SiC外延设备、高温MOCVD等设备关键件中，有效提高设备工艺能力和工艺稳定性。
附图说明
图1是本发明碳化硅薄壁结构件的制备方法的流程示意图。
图2是利用本发明的方法制备平面薄壁结构件的流程示意图。
图3是利用本发明的方法制备非平面异形薄壁结构件的流程示意图。
具体实施方式
以下结合说明书附图和具体实施例对本发明作进一步详细说明。
图1至图3示出了本发明的一种实施例，本实施例的碳化硅薄壁结构件的制备方法，包括以下步骤：
S1、利用石墨基材制作模具；
根据所要求制作的结构件的尺寸规划石墨模具的尺寸形状及加工，一般可为平面等厚薄板结构件，或者圆柱薄壁管、钟罩式坩埚、MOCVD托盘等非平面异形结构件；平面等厚薄板结构件尺寸规划是分别以石墨基材表面为基准，向外生长厚度为结构厚度尺寸，可以得到两个基准表面对称的两个结构件；非平面异形薄壁结构件尺寸规划可以以石墨基材内表面或外面为基准，向内或外生长厚度为结构厚度尺寸，取其中以相应基准面方向生长的结构件为最终获得；
S2、采用化学气相沉积法(CVD)在石墨基材表面生长碳化硅；
S3、从工件的边缘处切割碳化硅包裹部分使内部的石墨基材重新裸露出来；
S4、将工件中的石墨基材完全与氧气进行反应，获得固体碳化硅工件。
该碳化硅薄壁结构件的制备方法，采用全固态沉积碳化硅材料制作结构件，纯度最高可达99.9999％，Fe、Al、Cu、Zn等金属杂质可降至ppb(part per billion，十亿分比浓度)级别，结合碳化硅本身的材料特性，可有效地避免高温、污染、氧化、腐蚀、材料强度等问题，能广泛地应用于SiC氧化炉设备、SiC外延设备、高温MOCVD等设备关键件中，有效提高设备工艺能力和工艺稳定性。
进一步地，本实施例中，S2的详细步骤为：
S2.1、将石墨基材放入化学气相沉积设备内，并将化学气相沉积设备抽真空及置换气体；
S2.2、通入氮气，进行预热升温至600～800℃，升温速率1～15℃/min；
S2.3、通入氮气和氢气，继续升温至1400～1600℃，升温速率1～10℃/min；
S2.4、待温场稳定之后，开始通入原料气体三氯甲基硅烷(也可以是同类原料气体)、氢气和氩气，以10～200μm/h速率生进行生长。
更进一步地，本实施例中，S2的详细步骤还包括：
S2.5、待碳化硅厚度生长200～500μm时，降温，将工件旋转和/或倒置；
S2.6、重复步骤S2.1至2.5，直到碳化硅总生长厚度达到目标要求。也即采用多次重复生长的方式，每次生长之后对工件进行旋转一定角度、倒置，有利于工件同一表面碳化硅薄膜各处保持均匀以及工件内外两表面碳化硅薄膜保持均匀一致。
更进一步地，本实施例中，步骤S4中，将工件放入高温氧化炉中，升温至900～1200℃，通入氧气，使石墨基材在高温下与氧气进行反应，生成二氧化碳排出，待石墨基材完全反应后获得固体碳化硅工件。
进一步地，本实施例中，碳化硅薄壁结构件的制备方法还包括步骤：
S5、根据目标尺寸和表面形貌要求，对固体碳化硅工件进行抛光、打磨和二次尺寸调整。
更进一步地，本实施例中，碳化硅薄壁结构件的制备方法还包括步骤：
S6、采用10％浓度的氢氟酸进行清洗，然后利用超声波进行去离子水洗，获得成品。
进一步地，本实施例中，步骤S1中，石墨基材的厚度为2-50㎜，表面光洁度在500-1000nm，加工成模具后进行纯化处理，例如高温纯化处理等。
虽然本发明已以较佳实施例揭露如上，然而并非用以限定本发明。任何熟悉本领域的技术人员，在不脱离本发明技术方案范围的情况下，都可利用上述揭示的技术内容对本发明技术方案做出许多可能的变动和修饰，或修改为等同变化的等效实施例。因此，凡是未脱离本发明技术方案的内容，依据本发明技术实质对以上实施例所做的任何简单修改、等同变化及修饰，均应落在本发明技术方案保护的范围内。
Claims (8)
1.一种碳化硅薄壁结构件的制备方法，其特征在于：包括以下步骤：
S1、利用石墨基材制作模具；
S2、采用化学气相沉积法在石墨基材表面生长碳化硅；
S3、从工件的边缘处切割碳化硅包裹部分使内部的石墨基材重新裸露出来；
S4、将工件中的石墨基材完全与氧气进行反应，获得固体碳化硅工件。
2.根据权利要求1所述的碳化硅薄壁结构件的制备方法，其特征在于：S2的详细步骤为：
S2.1、将石墨基材放入化学气相沉积设备内，并将化学气相沉积设备抽真空及置换气体；
S2.2、通入氮气，进行预热升温至600～800℃，升温速率1～15℃/min；
S2.3、通入氮气和氢气，继续升温至1400～1600℃，升温速率1～10℃/min；
S2.4、待温场稳定之后，开始通入原料气体、氢气和氩气，以10～200μm/h速率生进行生长。
3.根据权利要求2所述的碳化硅薄壁结构件的制备方法，其特征在于：S2的详细步骤还包括：
S2.5、待碳化硅厚度生长200～500μm时，降温，将工件旋转和/或倒置；
S2.6、重复步骤S2.1至2.5，直到碳化硅总生长厚度达到目标要求。
4.根据权利要求2所述的碳化硅薄壁结构件的制备方法，其特征在于：步骤S2.4中原料气体为三氯甲基硅烷。
5.根据权利要求1所述的碳化硅薄壁结构件的制备方法，其特征在于：步骤S4中，将工件放入高温氧化炉中，升温至900～1200℃，通入氧气，使石墨基材在高温下与氧气进行反应，生成二氧化碳排出，待石墨基材完全反应后获得固体碳化硅工件。
6.根据权利要求1至5中任一项所述的碳化硅薄壁结构件的制备方法，其特征在于：还包括步骤：
S5、根据目标尺寸和表面形貌要求，对固体碳化硅工件进行抛光、打磨和二次尺寸调整。
7.根据权利要求6所述的碳化硅薄壁结构件的制备方法，其特征在于：还包括步骤：
S6、采用10％浓度的氢氟酸进行清洗，然后利用超声波进行去离子水洗，获得成品。
8.根据权利要求1至5中任一项所述的碳化硅薄壁结构件的制备方法，其特征在于：步骤S1中，石墨基材的厚度为2-50㎜，表面光洁度在500-1000nm，加工成模具后进行纯化处理。
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