CN112876228A - 一种高模量堇青石基低热膨胀陶瓷及其制备方法 - Google Patents
一种高模量堇青石基低热膨胀陶瓷及其制备方法 Download PDFInfo
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- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 41
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 41
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Abstract
本发明公开了一种高模量堇青石基低热膨胀陶瓷，由以下重量分数的物质组成：堇青石高纯粉74.5％‑81％、热膨胀系数调节剂7‑15％、弹性模量调节剂2.5％‑9％和助烧剂0.5‑1.5％。本发明的有益效果是：本发明高模量堇青石基低热膨胀陶瓷致密性较好，其致密度≥97％，弹性模量≥140GPa；针对光刻机应用领域，本发明提拱了一种光刻机操作温度下(20℃附近温度点)具备超低热膨胀系数的高模量堇青石基陶瓷材料制备方法，整体制备工艺简单，易操作，成本较低，易于实现产业化。
Description
技术领域
本发明涉及精密半导体部件用陶瓷的制备，具体涉及一种高模量堇青石基低热膨胀陶瓷及其制备方法。
背景技术
光刻机是极大规模集成电路制备工艺中的关键设备，目前的光刻工艺技术已逐渐向线宽28nm/22nm，甚至16nm的方向转移，对于移动平台材料的选择要求极其苛刻，满足特定性能要求的移动平台的材料开发成了制约光刻技术实施的瓶颈技术。光刻机要达到预定的精度和生产效率，要求作为移动平台的结构材料，既要满足其本身尺寸稳定、重量轻，还要实现在高速移动时保持精确定位；因此材料须具有高刚性、低密度、低热膨胀的特性。作为精密半导体部件的低热膨胀陶瓷材料，堇青石陶瓷因其优异的抗热震性，以及较高的机械强度和抗化学腐蚀能力而备受关注，且全球最大的半导体巨头ASML早已将其应用到高端光刻机平台材料中，而我国的半导体行业起步较晚，至今仍在研发阶段，因此开发一种高模量的堇青石基低热膨胀陶瓷，从根本上解决平台结构轻量化的问题，满足结构设计要求，满足光刻精度的需求，成为高精密半导体部件研发的关键。
发明内容
本发明针对精密半导体用低热膨胀陶瓷致密性差以及模量低等问题，提供一种高模量堇青石基低热膨胀陶瓷，由以下重量分数的物质组成：堇青石高纯粉74.5％-81％、热膨胀系数调节剂7-15％、弹性模量调节剂2.5％-9％和助烧剂0.5-1.5％。
具体地，所述所述热膨胀系数调节剂为高纯氧化镁、氧化铝以及氧化硅按照堇青石标准配比组成的混合体系；所述弹性模量调节剂Si3N4粉；所述助烧剂为ZrO2和Y2O3的混合物。
进一步，本发明高模量堇青石基低热膨胀陶瓷的制备方法为：
1)按重量分数称取各组分，将高纯堇青石粉体、弹性模量调节剂及热膨胀系数调节剂混合，置于球磨罐中进行球磨后手动造粒，过筛，获得流动性良好的造粒粉体；
2)将造粒粉体先采用模压预成型，后借助冷等静压相方式获得无缺陷坯件；
3)将步骤2)所得坯件进行固化处理；
4)将步骤3)固化处理后的坯件置于热压烧结炉中进行烧结，降温后即得。
在上述方法中，步骤2)冷等静压参数为60MPa/15s-200MPa/30s；步骤3)固化温度为150-200℃，时间为8-12h；步骤4)热压烧结温度为1360-1370℃，保温时间1h。
本发明的有益效果是：本发明高模量堇青石基低热膨胀陶瓷致密性较好，其致密度≥97％，弹性模量≥140GPa；针对光刻机应用领域，本发明提拱了一种光刻机操作温度下(20℃附近温度点)具备超低热膨胀系数的高模量堇青石基陶瓷材料制备方法，整体制备工艺简单，易操作，成本较低，易于实现产业化。
附图说明
图1为实施例1中不同测试温度点的平均热膨胀系数。
具体实施方式
以下结合实例对本发明进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
一种高模量堇青石基低热膨胀陶瓷的制备方法，包括以下步骤：
①将81wt％高纯堇青石粉体、2.5wt％Si3N4粉、15wt％堇青石生料以及1.5wt％ZrO2-Y2O3组成的混合物置于球磨罐中，在酒精介质以及研磨球作用下均匀混合后进行手动造粒，过筛，获得流动性良好的造粒粉体；
②将造粒粉体先采用模压预成型，后借助冷等静压相方式获得无缺陷成型样品，模压成型工艺为60MPa/15s，冷等静压成型工艺为200MPa/30s；
③将步骤②中获得的样品置于恒温干燥箱中于150℃保温12h，进行充分的固化；
④将固化处理后的样品置于热压烧结炉中，于1370℃/1h烧结工艺条件下进行烧结，降温后即得。
实施例1获得的堇青石基低热膨胀陶瓷致密度为97.2％，弹性模量为141GPa，20℃附近点平均热膨胀系数为3*10-8，此工艺添加Si3N4作为复相成分，增强了比刚度的同时，提高耐磨损程度，仍然保持了超低热膨胀特性。
实施例2
一种高模量堇青石基低热膨胀陶瓷的制备方法，包括以下步骤：
①将78.5wt％高纯堇青石粉体、5wt％Si3N4粉、15wt％堇青石生料以及1.5wt％ZrO2-Y2O3组成的混合物置于球磨罐中，在酒精介质以及研磨球作用下均匀混合后进行手动造粒，过筛，获得流动性良好的造粒粉体；
②将造粒粉体先采用模压预成型，后借助冷等静压相方式获得无缺陷成型样品，模压成型工艺为60MPa/15s，冷等静压成型工艺为200MPa/30s；
③将步骤②中获得的样品置于恒温干燥箱中于150℃保温12h，进行充分的固化；
④将固化处理后的样品置于热压烧结炉中，于1350℃/1h烧结工艺条件下进行烧结，降温后即得。
实施例2获得的堇青石基低热膨胀陶瓷致密度为94.5％，弹性模量为114GPa，20℃附近点平均热膨胀系数为8*10-7，氮化硅含量虽然增加，但由于温度的降低，致密度下降，弹性模量随之降低。
实施例3
一种高模量堇青石基低热膨胀陶瓷的制备方法，包括以下步骤：
①将78.5wt％高纯堇青石粉体、5wt％Si3N4粉、15wt％堇青石生料以及1.5wt％ZrO2-Y2O3组成的混合物置于球磨罐中，在酒精介质以及研磨球作用下均匀混合后进行手动造粒，过筛，获得流动性良好的造粒粉体；
②将造粒粉体先采用模压预成型，后借助冷等静压相方式获得无缺陷成型样品，模压成型工艺为60MPa/15s，冷等静压成型工艺为200MPa/30s；
③将步骤②中获得的样品置于恒温干燥箱中于150℃保温12h，进行充分的固化；
④将固化处理后的样品置于热压烧结炉中，于1370℃/1h烧结工艺条件下进行烧结，降温后即得；
实施例3获得的堇青石基低热膨胀陶瓷致密度为97.6％，弹性模量为145GPa，20℃附近点平均热膨胀系数为6*10-8。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种高模量堇青石基低热膨胀陶瓷，其特征在于，由以下重量分数的物质组成：
堇青石高纯粉74.5％-81％、热膨胀系数调节剂7-15％、弹性模量调节剂2.5％-9％和助烧剂0.5-1.5％。
2.根据权利要求1所述的高模量堇青石基低热膨胀陶瓷，其特征在于，所述热膨胀系数调节剂为高纯氧化镁、氧化铝以及氧化硅按照堇青石标准配比组成的混合体系。
3.根据权利要求1所述的高模量堇青石基低热膨胀陶瓷，其特征在于，所述弹性模量调节剂Si3N4粉。
4.根据权利要求1所述的高模量堇青石基低热膨胀陶瓷，其特征在于，所述助烧剂为ZrO2和Y2O3的混合物。
5.一种如权利要求1-4任一项所述的高模量堇青石基低热膨胀陶瓷的制备方法，其特征在于，包括以下步骤：
1)按重量分数称取各组分，将高纯堇青石粉体、弹性模量调节剂及热膨胀系数调节剂混合，置于球磨罐中进行球磨后手动造粒，过筛，获得流动性良好的造粒粉体；
2)将造粒粉体先采用模压预成型，后借助冷等静压相方式获得无缺陷坯件；
3)将步骤2)所得坯件进行固化处理；
4)将步骤3)固化处理后的坯件置于热压烧结炉中进行烧结，降温后即得。
6.根据权利要求5所述的方法，其特征在于，步骤2)中冷等静压参数为60MPa/15s-200MPa/30s。
7.根据权利要求5所述的方法，其特征在于，步骤3)中固化温度为150-200℃，时间为8-12h。
8.根据权利要求5所述的方法，其特征在于，步骤4)中热压烧结温度为1360-1370℃，保温时间1h。
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