CN114409407A - 一种半导体悬臂桨产品的碳化硅含量提纯、提升方法 - Google Patents
一种半导体悬臂桨产品的碳化硅含量提纯、提升方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000004065 semiconductor Substances 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 22
- 239000011265 semifinished product Substances 0.000 claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 235000015895 biscuits Nutrition 0.000 claims abstract description 10
- 239000011368 organic material Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 238000005488 sandblasting Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims abstract description 4
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 4
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 238000007569 slipcasting Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012752 auxiliary agent Substances 0.000 claims description 12
- 239000006229 carbon black Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920005591 polysilicon Polymers 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000011856 silicon-based particle Substances 0.000 claims description 3
- 238000005475 siliconizing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical group O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
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- 239000011148 porous material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，碳化硅原料使用硝酸、氢氟酸、盐酸进行酸洗提纯,烘干；采用有机材质的搅拌锅搅拌原料得到合适的浆料；注浆模具配合的工装表面进行封装，浆料注浆入到处理好的注浆模具中；注浆成型后，干燥后脱模成素坯，修整采用碳化硅砂纸处理；胚体装炉烧结得到碳化硅悬臂桨半成品；出炉后的碳化硅悬臂桨半成品不打磨，使用碳化硅颗粒、干冰进行喷砂处理，将步骤7）处理好的碳化硅悬臂桨半成品通入高纯一甲基三氯硅烷，沉淀形成CVD涂层，得到成品碳化硅悬臂桨。少了金属杂质的引入，提高产品的强度，避免脆断的发生，有效的延长了产品的使用寿命，同时由于减少了金属杂质，可使用于半导体产品中。
Description
技术领域
本发明属于碳化硅材料技术领域，具体涉及一种半导体悬臂桨产品的碳化硅含量提纯、提升方法。
背景技术
悬臂桨是设备中晶圆装载系统的关键部件，可以保证晶圆与炉管的同心度，进而使扩散、氧化更均匀。特别是碳化硅悬臂桨具有高强度、高纯度、高导热、无气孔、耐酸碱腐蚀、高温下无污染、不变形及良好的抗热震稳定性、载重量大等特点，避免了与炉管的直接接触，延长了炉管的使用寿命，解决了其它材质悬臂桨易断裂，载重量小，成本高的问题。
碳化硅悬臂桨包括三个部分，即固定区、过渡区和负载区。其中，固定区是空心并且是带有圆角的方形管，断面可以是正方形；也可以是长方形，现有技术中碳化硅悬臂桨的制作工艺有多种，但碳化硅悬臂桨的合格率并不高，由于悬臂桨产品中碳化硅含量不纯，导致制得的碳化硅悬臂桨存在强度低等问题，尤其在Si扩散的同时会伴随空洞出现，导致渗硅层内有许多孔隙，渗层不致密，严重影响碳化硅悬臂桨的使用。
发明内容
为了克服上述现有技术的不足，本发明的目的是提供一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，现有注浆产品还有少量金属杂质，会在高温使用过程中发生脆断，同时不能用于半导体产品中，本发明发减少了金属杂质的引入，提高产品的强度，避免脆断的发生，有效的延长了产品的使用寿命，同时由于减少了金属杂质，可使用于半导体产品中。
为了实现上述目的，本发明采用的技术方案是：
一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，包括以下步骤：
步骤1、碳化硅原料使用硝酸、氢氟酸、盐酸进行酸洗提纯,采用有机材质的搅拌棒搅拌，待原料和酸充分反应，杂质酸化掉之后，进行烘干，其中碳化硅原料在硝酸池子浸泡12-48h后,再在氢氟酸池子24-48h、然后再盐酸1-12h；
步骤2、采用有机材质的搅拌锅搅拌处理后的碳化硅原料、炭黑、助剂，得到合适的浆料；浆料制备工艺为：水中分别加入三次助剂，每次搅拌10-30分钟后，然后加入炭黑，搅拌20-50分钟后，依次加入不同颗粒大小的三种碳化硅，边加入边搅拌，搅拌24-48小时，并检测粘度，不符合继续加入水，合格后备用；
步骤3、注浆模具配合的工装及注浆后转移素胚的转移工具整体进行封装，采用聚氯乙烯薄膜包裹，待用；
步骤4、将步骤2）搅拌合适的浆料注浆入到处理好的注浆模具中；
步骤5、注浆成型后脱模，放置在步骤3）准备好的工装上，由转移工具转移到烘房进行烘干处理，干燥采用碳化硅砂纸修整素胚；
步骤6、步骤5）得到的素胚装炉烧结，烧结过程使用多晶硅渗硅，经恒温、降温，得到碳化硅悬臂桨半成品；
步骤7、出炉后的碳化硅悬臂桨半成品不打磨，使用碳化硅颗粒或干冰进行喷砂处理，直到表面没有多余硅；所述的碳化硅颗粒喷砂处理为将表面处理后的单质硅颗粒均匀铺洒到碳化硅悬臂桨半成品的表面，提高碳化硅的均一性；
步骤8、将步骤7）处理好的碳化硅悬臂桨半成品通入高纯一甲基三氯硅烷，沉淀形成CVD涂层，得到成品碳化硅悬臂桨。
所述的烧结炉膛内石墨件均使用成本更高的高纯石墨件，且单炉单用。
所述的有机材质采用硬质塑料。
所述的碳化硅颗粒为表面处理的多晶硅，纯度99.99%。
所述的浆料中成分按质量分数比为：水分15-30份、碳化硅70-80份、炭黑5-6份、助剂0.1-2份。
所述的助剂为氧化钇。
本发明的有益效果是：
现有注浆产品还有少量金属杂质，会在高温使用过程中发生脆断，同时不能用于半导体产品中，本发明发减少了金属杂质的引入，提高产品的强度，避免脆断的发生，合格率100%，有效的延长了产品的使用寿命，同时由于减少了金属杂质，可使用于半导体产品中。
具体实施方式
以下结合法实施例对本发明进一步叙述。
一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，包括以下步骤：
步骤1、碳化硅原料使用硝酸、氢氟酸、盐酸进行酸洗提纯,采用有机材质的搅拌棒搅拌，待原料和酸充分反应，杂质酸化掉之后，进行烘干，其中碳化硅原料在硝酸池子浸泡12-48h后,再在氢氟酸池子24-48h、然后再盐酸1-12h；
步骤2、采用有机材质的搅拌锅搅拌处理后的碳化硅原料、炭黑、助剂，得到合适的浆料；浆料制备工艺为：水中分别加入三次助剂，每次搅拌10-30分钟后，然后加入炭黑，搅拌20-50分钟后，依次加入不同颗粒大小的三种碳化硅，边加入边搅拌，搅拌24-48小时，并检测粘度，不符合继续加入水，合格后备用；
步骤3、注浆模具配合的工装及注浆后转移素胚的转移工具整体进行封装，采用聚氯乙烯薄膜包裹，待用；
步骤4、将步骤2）搅拌合适的浆料注浆入到处理好的注浆模具中；
步骤5、注浆成型后脱模，放置在步骤3）准备好的工装上，由转移工具转移到烘房进行烘干处理，干燥采用碳化硅砂纸修整素胚；
步骤6、步骤5）得到的素胚装炉烧结，烧结过程使用多晶硅渗硅，经恒温、降温，得到碳化硅悬臂桨半成品；
步骤7、出炉后的碳化硅悬臂桨半成品不打磨，使用碳化硅颗粒或干冰进行喷砂处理，直到表面没有多余硅；所述的碳化硅颗粒喷砂处理为将表面处理后的单质硅颗粒均匀铺洒到碳化硅悬臂桨半成品的表面，提高碳化硅的均一性；
步骤8、将步骤7）处理好的碳化硅悬臂桨半成品通入高纯一甲基三氯硅烷，沉淀形成CVD涂层，得到成品碳化硅悬臂桨。
所述的烧结炉膛内石墨件均使用成本更高的高纯石墨件，且单炉单用。
所述的有机材质采用硬质塑料。
所述的碳化硅颗粒为表面处理的多晶硅，纯度99.99%。
所述的浆料中成分按质量分数比为：水分15-30份、碳化硅70-80份、炭黑5-6份、助剂0.1-2份。
所述的助剂为氧化钇。
实施例
对产品中元素检测如下表：
产品性能对比，样品1、样品2、样品3，样品1不做处理直接烘干，样品2不做喷砂及CVD涂层处理，样品3按上述步骤处理。
检测结果，弯曲强度如下：样品1均值255MPa，样品2均值266MPa，样品3均值276MPa。
Claims (6)
1.一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，包括以下步骤：
步骤1、碳化硅原料使用硝酸、氢氟酸、盐酸进行酸洗提纯,采用有机材质的搅拌棒搅拌，待原料和酸充分反应，杂质酸化掉之后，进行烘干，其中碳化硅原料在硝酸池子浸泡12-48h后,再在氢氟酸池子24-48h、然后再盐酸1-12h；
步骤2、采用有机材质的搅拌锅搅拌处理后的碳化硅原料、炭黑、助剂，得到合适的浆料；浆料制备工艺为：水中分别加入三次助剂，每次搅拌10-30分钟后，然后加入炭黑，搅拌20-50分钟后，依次加入不同颗粒大小的三种碳化硅，边加入边搅拌，搅拌24-48小时，并检测粘度，不符合继续加入水，合格后备用；
步骤3、注浆模具配合的工装及注浆后转移素胚的转移工具整体进行封装，采用聚氯乙烯薄膜包裹，待用；
步骤4、将步骤2）搅拌合适的浆料注浆入到处理好的注浆模具中；
步骤5、注浆成型后脱模，放置在步骤3）准备好的工装上，由转移工具转移到烘房进行烘干处理，干燥采用碳化硅砂纸修整素胚；
步骤6、步骤5）得到的素胚装炉烧结，烧结过程使用多晶硅渗硅，经恒温、降温，得到碳化硅悬臂桨半成品；
步骤7、出炉后的碳化硅悬臂桨半成品不打磨，使用碳化硅颗粒或干冰进行喷砂处理，直到表面没有多余硅；所述的碳化硅颗粒喷砂处理为将表面处理后的单质硅颗粒均匀铺洒到碳化硅悬臂桨半成品的表面，提高碳化硅的均一性；
步骤8、将步骤7）处理好的碳化硅悬臂桨半成品通入高纯一甲基三氯硅烷，沉淀形成CVD涂层，得到成品碳化硅悬臂桨。
2.根据权利要求1所述的一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，其特征在于，所述的烧结炉膛内石墨件均使用成本更高的高纯石墨件，且单炉单用。
3.根据权利要求1所述的一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，其特征在于，所述的有机材质采用硬质塑料。
4.根据权利要求1所述的一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，其特征在于，所述的碳化硅颗粒为表面处理的多晶硅，纯度99.99%。
5.根据权利要求1所述的一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，其特征在于，所述的浆料中成分按质量分数比为：水分15-30份、碳化硅70-80份、炭黑5-6份、助剂0.1-2份。
6.根据权利要求1所述的一种半导体悬臂桨产品的碳化硅含量提纯、提升方法，其特征在于，所述的助剂为氧化钇。
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