CN116332647A - 抗等离子体稀土氧化物固溶体陶瓷及其制造方法 - Google Patents
抗等离子体稀土氧化物固溶体陶瓷及其制造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 239000006104 solid solution Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 238000003746 solid phase reaction Methods 0.000 claims description 5
- 238000001513 hot isostatic pressing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 abstract description 8
- 239000011224 oxide ceramic Substances 0.000 abstract description 7
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 235000015895 biscuits Nutrition 0.000 description 10
- 230000007547 defect Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000009694 cold isostatic pressing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000001020 plasma etching Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
抗等离子体的稀土氧化物固溶体陶瓷,所陶瓷包括:不少于80mol%的Er2O3,不多于20mol%的Y2O3;以及相对于上述两种物质重量之和的0.1‑1.0wt%的ZrO2、TiO2、Gd2O3、MgO或者0.01‑0.1wt%SiO2中的至少一种。本发明的陶瓷具有比现有的氧化铝陶瓷、氧化钇陶瓷及氧化铒陶瓷具有更好的抗等离子体性能。
Description
技术领域
本发明属于稀土氧化物类陶瓷材料。
背景技术
在半导体制造领域,等离子体蚀刻和等离子体清洁工艺是处理衬底重要手段。等离子体可能具有高度腐蚀性,并且可能腐蚀处理室和暴露于等离子体的其他表面。这种腐蚀可能会产生颗粒,这些颗粒经常会污染正在处理的基板,从而导致器件缺陷。此外,腐蚀可能导致来自腔室组件的金属原子污染处理过的晶片。
随着半导体制造水平和要求不断提高,对颗粒污染物和金属原子的污染更加敏感。因此,颗粒缺陷和金属污染的允许水平可能会不断降低。为了解决等离子蚀刻或等离子清洁工艺引入的颗粒缺陷和金属污染,已经开发出耐等离子的腔室材料。这些抗等离子材料包括由Al2O3、A1N、SiC和Y2O3组成的陶瓷。然而,这些陶瓷材料的抗等离子特性可能不足以满足某些应用。例如,使用传统陶瓷制造的抗等离子陶瓷盖和喷嘴在用于具有20nm或更小的关键尺寸的半导体器件的等离子体蚀刻工艺时,制造工艺可能会产生不可接受的颗粒缺陷水平。因此,开发具有更好抗等离子体性能的陶瓷材料,成为半导体制造领域的一项重要的事情。
发明内容
本发明提出一种稀土氧化物固溶体陶瓷材料,从而获得更好的抗等离子体性能,以满足等离子体蚀刻和等离子体清洁工艺的更高需求。
本发明的稀土氧化物固溶体陶瓷材料表达为ErxY(2-x)O3,其中0.1≤x≤0.4。为了促进高温烧结致密化,本发明的稀土氧化物固溶体陶瓷还添加ErxY(2-x)O3重量的0.1-1.0wt%的ZrO2、Gd2O3、TiO2、MgO或者0.01-0.1wt%SiO2中的至少一种作为助剂。
本发明还公开了稀土氧化物固溶体陶瓷材料的制造方法,以Er2O3和Y2O3作为原料,添加助剂后通过高温固相反应合成ErxY(2-x)O3固溶体粉体,再高温烧结得到本发明的稀土氧化物固溶体陶瓷。
本发明的另一种优选方案是以Er2O3和Y2O3粉为原料,并添加适当的助剂,通过反应烧结得到ErxY(2-x)O3固溶体陶瓷。
优选地,本发明的稀土氧化物固溶体陶瓷是在真空或氢气气氛下高温烧结,烧结温度为1700-1850℃。本发明的优选方案,还包括采用热等静压实现致密化,热等静压温度为1700-1750℃,以及退火处理消除氧空位。
本发明以氧化铝陶瓷、氧化钇陶瓷及氧化铒陶瓷作为对比,在相同条件下进行抗等离子体性能测试,用于评价本发明的陶瓷的抗等离子体性能。
有益效果
本发明的稀土氧化物固溶体陶瓷比现有的氧化铝陶瓷、氧化钇陶瓷及氧化铒陶瓷具有更好的抗等离子体性能。
具体实施方式
下面结合实施例对本发明做进一步详细具体的说明。
有必要在此指出:以下实施例只用于对本发明做进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述实施例中具体的原料配比、烧结温度和保温时间等仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适范围内的选择,而并非要限定于下文示例的具体数值。
实施例1-5给出了本发明稀土氧化物固溶体陶瓷的具体实施过程。所得陶瓷经过研磨和化学机械抛光后,用CHF3/CF4化学品所产生的等离子体进行抗侵蚀性能测试。通过测量侵蚀厚度与侵蚀时间的比值,计算侵蚀速度。并且与采用现有技术制造的Al2O3、Y2O3及Er2O3陶瓷的抗等离子体性能一同试验,以Al2O3陶瓷的侵蚀速度为基准,进行归一化处理。所得结果见表1。
实施例1
按照x=0.4的比例,设计组成Er0.4Y1.6O3的固溶体。以纯度不小于99.9%的Er2O3和Y2O3粉为原料,按照前述比例称取两种粉体,并添加总重量0.5wt%的ZrO2粉,采用湿法球磨的方法获得平均粒径小于500nm的混合粉体。将所得粉体过200目筛后,采用冷等静压成型技术200MPa压制成素坯。将素坯在真空度优于5*10-3Pa的真空钨丝炉中烧结,以10℃/min的速度升温至1780℃保温8h,然后升温至1840℃保温25h。所得陶瓷在1000℃的空气气氛中处理10h,以消除真空引起的氧缺陷。测得归一化的等离子体侵蚀速度为0.29。
实施例2
按照x=0.2的比例,设计组成Er0.2Y1.8O3的固溶体。以纯度不小于99.9%的Er2O3和Y2O3粉为原料,按照前述比例称取两种粉体,并添加总重量的0.1wt%的TiO2粉,采用湿法球磨的方法获得平均粒径小于500nm的混合粉体。将所得粉体经过200目筛后,采用冷等静压成型技术200MPa压制成素坯。将素坯在空气气氛炉中以2℃/min的速度升温至在1750℃保温4h获得固溶体陶瓷预烧体。将预烧体在1700℃的热等静压炉中处理3h,压力介质为高纯Ar气体。所得陶瓷在1000℃的空气气氛中处理10h,以消除真空引起的氧缺陷。测得归一化的等离子体侵蚀速度为0.26。
实施例3
按照x=0.2的比例,设计组成Er0.2Y1.8O3的固溶体。以纯度不小于99.9%的Er2O3和Y2O3粉为原料,按照前述比例称取两种粉体,并添加总重量的0.05wt%的SiO2粉,采用湿法球磨的方法获得平均粒径小于500nm的混合粉体。将所得粉体经过200目筛后,采用冷等静压成型技术200MPa压制成素坯。将素坯在真空炉中以2℃/min的速度升温至在1780℃保温4h获得固溶体陶瓷预烧体。将预烧体在1750℃的热等静压炉中处理8h,压力介质为高纯Ar气体。所得陶瓷在1000℃的空气气氛中处理10h,以消除真空引起的氧缺陷。测得归一化的等离子体侵蚀速度为0.22。
实施例4
按照x=0.3的比例,设计组成Er0.3Y1.7O3的固溶体。以纯度不小于99.9%的Er2O3和Y2O3粉为原料,按照前述比例称取两种粉体,并添加总重量的1.0wt%的Gd2O3粉,采用湿法球磨的方法获得平均粒径小于500nm的混合粉体。将所得粉体经1100℃煅烧进行固相反应后,过200目筛,然后采用冷等静压成型技术200MPa压制成素坯。将素坯在真空度优于5*10- 3Pa的真空钨丝炉中烧结,以5℃/min的速度升温至在1800℃保温20h获得固溶体陶瓷。所得陶瓷在1000℃的空气气氛中处理10h,以消除真空引起的氧缺陷。测得归一化的等离子体侵蚀速度为0.28。
实施例5
按照x=0.1的比例,设计组成Er0.1Y1.9O3的固溶体。以纯度不小于99.9%的Er2O3和Y2O3粉为原料,按照前述比例称取两种粉体,并添加总重量的0.4wt%的ZrO2粉和0.2wt%的MgO粉,采用湿法球磨的方法获得平均粒径小于500nm的混合粉体。将所得粉体经1200℃煅烧进行固相反应后过200目筛,然后采用冷等静压成型技术200MPa压制成素坯。将素坯在真空度优于5*10-3Pa的真空钨丝炉中烧结,以8℃/min的速度升温至在1850℃保温25h获得固溶体陶瓷。所得陶瓷在1000℃的空气气氛中处理10h,以消除真空引起的氧缺陷。测得归一化的等离子体侵蚀速度为0.35。
表1等离子体对材料的侵蚀速度比较
Claims (7)
1.一种稀土氧化物固溶体陶瓷,具有良好的抗等离子体性能,其特征在于所述固溶体为ErxY(2-x)O3,其中0.1≤x≤0.4,添加重量的0.1-1.0wt%的ZrO2、TiO2、Gd2O3、MgO或者0.01-0.1wt%SiO2中的至少一种作为助剂。
2.一种制造如权利要求1所述的稀土氧化物固溶体陶瓷的方法,其特征在于以Er2O3和Y2O3作为原料,添加助剂后通过高温固相反应合成ErxY(2-x)O3固溶体粉体,再高温烧结得到本发明的稀土氧化物固溶体陶瓷。
3.如权利要求2所述的方法,其特征在于所述高温固相反应的温度是1100-1200℃。
4.如权利要求2所述的方法,其特征在于所述高温烧结在是1700-1850℃的真空炉中进行。
5.一种制造如权利要求1所述的稀土氧化物固溶体陶瓷的方法,其特征在于以Er2O3和Y2O3作为原料,添加助剂后通过反应烧结获得ErxY(2-x)O3固溶体陶瓷。
6.如权利要求5所述的方法,其特征在于所述反应烧结在是1700-1850℃的真空炉中进行或者在1700-1750℃的热等静压中完成。
7.如权利要求2-6的任意一项所述的方法,其特征在于所得稀土氧化物固溶体陶瓷还需要在1000℃的空气中进行退火。
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