CN111620701B - 一种多层复合陶瓷盘及其制造方法 - Google Patents

一种多层复合陶瓷盘及其制造方法 Download PDF

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CN111620701B
CN111620701B CN202010234112.9A CN202010234112A CN111620701B CN 111620701 B CN111620701 B CN 111620701B CN 202010234112 A CN202010234112 A CN 202010234112A CN 111620701 B CN111620701 B CN 111620701B
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ceramic
layer
sintered
metal electrode
piece
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CN111620701A (zh
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张巨先
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Yantai Rui Porcelain New Material Technology Co ltd
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Yantai Rui Porcelain New Material Technology Co ltd
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Priority to CN202010234112.9A priority Critical patent/CN111620701B/zh
Publication of CN111620701A publication Critical patent/CN111620701A/zh
Priority to JP2022556137A priority patent/JP7573641B2/ja
Priority to KR1020227033113A priority patent/KR20220144859A/ko
Priority to US17/912,046 priority patent/US20230140614A1/en
Priority to EP21775036.3A priority patent/EP4112584A4/en
Priority to PCT/CN2021/076782 priority patent/WO2021190207A1/zh
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Abstract

一种多层复合陶瓷盘及其制造方法，涉及半导体和材料科学领域。所述复合陶瓷盘包括至少一个基础三明治结构，包括：用陶瓷粉体制备一个片状陶瓷素坯；把陶瓷素坯在低于烧结温度的预烧结温度下，进行预烧结，得到具有一定强度的预烧结陶瓷件；在预烧结陶瓷件的上表面上形成一金属电极层；将预烧结陶瓷件放入模具中，且覆有金属电极层的上表面朝上；在预烧结陶瓷件上表面提供一陶瓷前体层；沿着预烧结陶瓷件轴向方向在烧结温度下加压烧结成一体，所述预烧结陶瓷件经加压烧结形成第二陶瓷层，所述陶瓷前体层经加压烧结形成第一陶瓷层，其中，所述金属电极层位于所述第一陶瓷层和第二陶瓷层之间并与第一陶瓷层和第二陶瓷层形成一基础三明治结构。

Description

一种多层复合陶瓷盘及其制造方法
技术领域
本发明涉及半导体和材料科学领域，具体的，涉及半导体制造工艺中的一种多层复合陶瓷盘及其制造方法，尤其是静电吸盘(Electrostatic chuck，简称ESC)和陶瓷加热盘及其制造方法。
背景技术
多层复合陶瓷盘被广泛应用于半导体加工设备中，根据其具体功能和结构的差别，半导体加工领域中的多层复合陶瓷盘包括静电吸盘和陶瓷加热盘，其中有些静电吸盘还同时具有加热盘的功能。在半导体加工设备中，静电吸盘被用于通过静电引力实现对硅晶片(wafer)的平稳夹持，而陶瓷加热盘则被用于加热静电吸盘上所夹持的硅晶片以使其保持在特定的温度。多层复合陶瓷盘广泛应用在等离子和真空环境下，如刻蚀、PVD、CVD、离子植入等半导体工艺过程中。传统的多层复合陶瓷盘，包括静电吸盘和陶瓷加热盘，通常采用包括一层或多层金属电极层的多层复合陶瓷盘结构，其基础结构为由两层陶瓷介质层和夹在两层陶瓷介质层之间的金属电极层所形成的三明治结构。具体应用在半导体加工设备中的复合陶瓷盘可能包含多层陶瓷介质层以及分别位于相邻陶瓷介质层之间的金属电极层。
半导体加工工艺对抛光后的硅晶片表面粗糙度和平面度参数的要求极高，因此这也就对与之接触的复合陶瓷盘的表面粗糙度和平面度提出了极高的要求。并且，对于静电吸盘而言，表面绝缘介质层厚度的均匀度还决定了静电吸盘各部分静电引力均匀程度。此外，在刻蚀过程中，由于硅晶片表面温度微小的温差，都可能造成很大的刻蚀偏差，进而影响到晶片的刻蚀效果。同样的，陶瓷加热盘各层之间的厚度是否均匀一致也直接影响到硅晶片表面温度分布，并进而影响到半导体加工工艺的精度。因此，对包括静电吸盘和陶瓷加热盘在内的复合陶瓷盘的工艺要求就是其基础三明治结构的各层的厚度均匀，且陶瓷复合盘的表面平面度好。
为了制备平面度好、厚度均匀的多层复合陶瓷盘，包括静电吸盘和陶瓷加热盘，目前常用的方法有两种：其一是分层烧结方法，即上下两陶瓷层分开烧制加工后，将电极层烧结在其中一层陶瓷层基体上。然后，将各层封装连接形成该基础三明治结构并确保各层功能，其优点是各层加工条件不受其他层限制，方便保证各层加工质量。但这样成型的基础三明治结构中，两陶瓷层硬接触而将金属电极层夹在其间，所以封装连接后的陶瓷盘性能稳定性和可靠性较差；其二是整体烧结方法，即将三明治结构的三层结构分步成型后叠加在一起，然后共同烧结制造。由于采用整体烧结工艺，这样成型的基础三明治结构的两层陶瓷层被烧结成一体，因此，其优点是各层结合牢固可靠，但整体烧结的工艺难度大，难以确保各层的高平面度要求。
因此，亟待提供一种适应于半导体加工领域的平面度好、各层厚度均匀的多层复合陶瓷盘及其制备方法。
发明内容
本发明旨在提供一种适应于半导体加工领域的平面度好、各层厚度均匀的多层复合陶瓷盘及其制备方法。
为此，本发明提出一种工艺简单、方便、容易实现、易于工业化生产、生产效率高、成品率高、可靠性好的复合陶瓷盘的制备方法，利用此方法制备所得的多层复合陶瓷盘平面度好、各层厚度均匀。
在本发明的一个方面，本发明提供了一种平面度好、厚度均匀的、适合用作半导体加工工艺中的静电吸盘和/或陶瓷加热盘的多层复合陶瓷盘及其制备方法。
本发明一种多层复合陶瓷盘的制备方法，其特征在于，采用模具进行加压烧结，模具为石墨热压模具，即石墨圆柱外桶内配有两个独立同轴的石墨圆柱体，下部的为石墨模具底托，上部的为石墨模具压盖(未在图中体现)。
多层复合陶瓷盘包括至少一个基础三明治结构，所述的一个基础三明治结构包括第一陶瓷层、第二陶瓷层以及位于第一陶瓷层和第二陶瓷层之间的位于所述第一陶瓷层和第二陶瓷层之间的金属电极层；制备方法具体包括以下步骤：
(1)用陶瓷粉体制备一个片状陶瓷素坯；把陶瓷素坯在低于烧结温度的预烧结温度下，进行预烧结，得到具有一定强度的预烧结陶瓷件；
(2)在预烧结陶瓷件的上表面上制备一金属电极层；
(3)将预烧结陶瓷件放入模具中石墨模具底托上，且覆有金属电极层的上表面朝上，在预烧结陶瓷件上表面提供一陶瓷前体层，沿着预烧结陶瓷件轴向方向在烧结温度下加压烧结成一体；其中，预烧结陶瓷件经加压烧结形成第二陶瓷层，陶瓷前体层经加压烧结形成第一陶瓷层，金属电极层位于所述第一陶瓷层和第二陶瓷层之间并与第一陶瓷层和第二陶瓷层形成一体化，即得到一个基础三明治结构。
或进一步优选，所述复合陶瓷盘包括两个基础三明治结构，其中第二陶瓷层的下表面还成型有一个金属电极层和一个第一陶瓷层，共形成两个基础三明治结构五层复合陶瓷盘，五层结构依次为第一陶瓷层/金属电极层/第二陶瓷层/金属电极层/第一陶瓷层；其制备方法包括以下步骤：
(1)用陶瓷粉体制备一个片状陶瓷素坯；把陶瓷素坯在低于烧结温度的预烧结温度下，进行预烧结，得到具有一定强度的预烧结陶瓷件；
(2)在预烧结陶瓷件的上表面和下表面分别制备一金属电极层，得到带有双金属电极层的预烧结陶瓷件；
(3)将陶瓷前体层、带有双金属电极层的预烧结陶瓷件依次按照如下的上下层关系：陶瓷前体层/带有双金属电极层预烧结陶瓷件/陶瓷前体层同轴配备到模具中石墨模具底托上，然后沿着预烧结陶瓷件轴向方向在烧结温度下加压烧结成一体；其中，预烧结陶瓷件经加压烧结形成第二陶瓷层，陶瓷前体层经加压烧结形成第一陶瓷层；
上述所述两个基础三明治结构五层复合陶瓷盘制备中的两个陶瓷前体层相同或不同，对应的第一陶瓷层材料相同或不同。
步骤(1)所述预烧结陶瓷件，可耐水浸泡，并能够进行尺寸公差精度在0.03mm以内的车、铣、磨的精加工。步骤(1)所述片状陶瓷素坯的成型方法是等静压成型。
进一步优选，还包括在步骤(2)在预烧结陶瓷件的上表面上制备一金属电极层之前，对所述的预烧结陶瓷件进行精加工，使其平面度更好、厚度更均匀。将预烧结陶瓷件加工至平面度不大于0.03mm。
进一步优选，步骤(2)所述金属电极层通过丝网印刷工艺或者镀膜工艺成型到预烧结陶瓷件上。进一步优选所述金属电极层的平面度不大于0.03mm。
进一步优选，步骤(3)所述陶瓷前体层为均匀分布的陶瓷粉体，或预成型好的未烧结片状陶瓷坯体。进一步优选所述未烧结片状陶瓷坯体为采用陶瓷粉体在模具内预压成型的。
进一步优选，步骤(1)所述预烧结陶瓷件的预烧结温度比步骤(3)烧结温度低20℃-600℃，优选低100℃-400℃；步骤(3)所述的烧结温度为致密化烧结温度，不同的材料有不同的致密化烧结温度。
进一步优选，步骤(1)陶瓷粉体和步骤(3)所述陶瓷前体层的材料成分均选自氧化物、非氧化物中的一种或几种，其中氧化物选自氧化铝、氧化锆、镁铝尖晶石等中的一种或两种，非氧化物选自氮化铝、氮化硅、碳化硅等中的一种或两种。烧结之后第二陶瓷层和第一陶瓷层对应的为氧化物陶瓷、非氧化物陶瓷中的一种或几种，其中氧化物陶瓷选自氧化铝陶瓷、氧化锆陶瓷、镁铝尖晶石等中的一种或两种，非氧化物陶瓷选自氮化铝、氮化硅、碳化硅等中的一种或两种。
所述第一陶瓷层和第二陶瓷层的面积大于所述金属电极层的面积，金属电极层包覆在第一陶瓷层和第二陶瓷层之间，第一陶瓷层和第二陶瓷层外缘部分互相接触并经加压烧结成一体。
本发明提供了一种复合陶瓷盘的制备方法尤其适用于半导体加工工艺的多层复合陶瓷盘的制备方法。所述复合陶瓷盘适合于用作半导体加工工艺中的静电吸盘和/或加热盘。根据本发明的实施例，该复合陶瓷盘的平面度好、厚度均匀。与传统复合陶瓷盘的制备方法相比较，具有精度高、工艺简单、成品率高、加工简便等优点。
附图说明
图1为本发明的多层复合陶瓷盘的基础三明治结构示意图；
图2为本发明的多层复合陶瓷盘基础三明治结构的制备过程示意图；
图3为具有两个基础三明治结构的五层复合陶瓷盘结构示意图；
图4为图3所示五层复合陶瓷盘的制备过程示意图；
附图标记：
1、第二陶瓷层；2、金属电极层；3、第一陶瓷层；4、石墨模具底托；5、石墨模具外筒；6、预烧结陶瓷件；7、陶瓷前体层。
具体实施方式
为使本发明的上述目的、特征和优点能够更为明显易懂，下面结合附图对本发明的具体实施例做详细的说明。
半导体加工工艺中使用的静电吸盘和加热盘都属于多层复合陶瓷盘，其功能结构都具有典型的基础三明治结构。本发明提供了一种适合于用作半导体加工工艺中使用的静电吸盘和加热盘的多层复合陶瓷盘及其制备方法。图1为本发明多层复合陶瓷盘的基础三明治结构示意图，图2为本发明多层复合陶瓷盘的基础三明治结构的制备过程示意图。按以下流程：
1.将喷雾造粒好的氧化铝粉体，用冷等静压成型出直径300mm，厚5mm的片状陶瓷素坯，成型压力为200MPa；
2.将直径300mm、厚5mm的片状陶瓷素坯，在氧化气氛下，1200℃下保温1小时，进行预烧结从而得到片状氧化铝预烧结陶瓷件6，在本实施例中，预烧结温度设定为1200℃，预烧结的温度设定与后续加压烧结的烧结温度有关，通常预烧结温度应当比加压烧结的烧结温度低20℃到600℃，优选低100℃到400℃；
3.用数控平面磨床，对氧化铝预烧结陶瓷件6的平面进行平磨加工，使其平面度不大于0.03mm，理想情况下，不大于0.008mm；
4.用丝网印刷的方法，把金属钨膏剂印刷到精密加工后的氧化铝预烧结陶瓷件6的一个平面上得到金属电极层2，金属电极层2的平面度不大于0.03mm，在其他实施例中也可以选用镀膜工艺或者其他薄膜成型工艺在预烧结陶瓷件上形成所述金属电极层2，在本实施例中金属电极层的材料为钨，但并不限定为钨，其它适合于作为金属电极使用的金属材料也可选择；
5.如图2所示，第一步，将涂敷有金属电极层2的氧化铝预烧结陶瓷件6平稳地放在石墨模具底托4上，然后套上石墨模具外筒5，且覆有金属电极层2的预烧结陶瓷件1的上表面朝上。第二步，在预烧结陶瓷件6上提供一陶瓷前体层7，在本实施例中，所述陶瓷前体层为均匀分布的氧化铝粉体，在其它实施例中，所述陶瓷前体层7也可以是预成型好的未烧结的片状陶瓷坯体。第三步，沿着氧化铝预烧结陶瓷件6的轴向方向加压烧结，本实施例设定的烧结温度为1600℃，保温30分钟，压力为20MPa。
经加压烧结，所述预烧结陶瓷件6形成第二陶瓷层1，所述陶瓷前体层形7形成第一陶瓷层3，所述金属电极层2对应图1的金属电极层2，且位于所述第一陶瓷层3和第二陶瓷层1之间并与第一陶瓷层和第二陶瓷层形成一基础三明治结构。
本实施例中，陶瓷前体层7和预烧结陶瓷件6的材料是氧化铝，经加压烧结后得到的均为氧化铝陶瓷。在其他实施例中，陶瓷前体层7和预烧结陶瓷件6的材料也可以是以下材料的一种或几种：氧化铝、氧化锆、镁铝尖晶石、氮化铝、氮化硅、碳化硅。在其他实施例中，所述第一陶瓷层和第二陶瓷层是氧化铝、氧化锆、镁铝尖晶石等氧化物陶瓷中的一种或多种。在其他实施例中，所述第一陶瓷层和第二陶瓷层中的一种或多种是氮化铝、氮化硅、碳化硅等非氧化物陶瓷中的一种或多种。在其他实施例中，所述第一陶瓷层和第二陶瓷层中的一种或多种是复相陶瓷。
如图1所示，所述第一陶瓷层和第二陶瓷层的面积大于所述金属电极层的面积，且其外缘部分互相接触并经加压烧结成一体，并从而将所述金属电极层完全封装
实施例2
本发明的复合陶瓷盘还可以是包括两个基础三明治结构的五层结构复合陶瓷盘。图3为包括两个基础三明治结构的五层复合陶瓷盘的示意图；图4为复合包括两个基础三明治结构的五层复合陶瓷盘的制备过程示意图。如图3和图4所示：
1.将喷雾造粒好的氧化铝粉体，用冷等静压成型出直径300mm，厚5mm的片状陶瓷素坯，成型压力为200MPa；
2.将直径300mm、厚5mm的氧化铝片状陶瓷素坯，在氧化气氛下，1200℃下保温1小时，进行预烧结从而得到片状预烧结陶瓷件6；
3.用数控平面磨床，对预烧结的氧化铝预烧结陶瓷件6的平面进行平磨加工，其平面度不大于0.01mm，理想情况下，不大于0.008mm。
4.用丝网印刷的方法，把金属钨膏剂印刷到精密加工后的氧化铝预烧结陶瓷件6的上下两个平面上形成金属钨电极层2，印刷后的金属钨电极层平面度不大于0.01mm。
5.按照图4所示，第一步，将石墨模具外筒5套在石墨模具底托4上，然后在石墨模具底托4上提供一层陶瓷前体层7(此陶瓷前体层为均匀分布的氧化铝粉体，也可以是预成型好的未烧结的片状陶瓷坯体)。把两面涂敷有上金属电极层2的氧化铝陶瓷预烧件6平稳地放置在石墨模具底托上的陶瓷前体层上。第二步，在氧化铝陶瓷预烧件6上再提供一陶瓷前体层7(此陶瓷前体层为均匀分布的氧化铝粉体，也可以是预成型好的未烧结的片状陶瓷坯体)。第三步，沿着氧化铝陶瓷预烧件6轴向方向加压烧结，烧结温度设定为1600℃，保温30分钟，压力为20MPa。
同时参照图3和图4，经加压烧结，所述氧化铝陶瓷预烧件6形成第二陶瓷层1，所述两陶瓷前体层7均形成第一陶瓷层3，所述上金属电极层2对应于图3所示的五层复合陶瓷盘结构中的上金属电极层2，形成两个基础三明治结构。
本实施例中，陶瓷前体层、预烧结陶瓷件的材料是氧化铝，经加压烧结后得到的均为氧化铝陶瓷。在其他实施例中，陶瓷前体层和预烧结陶瓷件的材料也可以是以下材料的一种或几种：氧化铝、氧化锆、镁铝尖晶石、氮化铝、氮化硅、碳化硅。在其他实施例中，所述第一陶瓷层、第二陶瓷层是氧化铝、氧化锆、镁铝尖晶石等氧化物陶瓷中的一种或多种。在其他实施例中，所述第一陶瓷层、第二陶瓷层是氮化铝、氮化硅、碳化硅等非氧化物陶瓷中的一种或多种。在其他实施例中，所述第一陶瓷层、第二陶瓷层是一种或多种是复相陶瓷。
如图3所示，所述第一陶瓷层、第二陶瓷层的面积均大于所述金属电极层的面积，且第一陶瓷层、第二陶瓷层外缘部分两两互相接触并经加压烧结成一体，从而将金属电极层完全封装。
虽然本发明披露如上，但本发明并非限定于此。任何本领域技术人员，在不脱离本发明的精神和范围内，均可作各种更动与修改，因此本发明的保护范围应当以权利要求所限定的范围为准。

Claims (8)

1.一种多层复合陶瓷盘的制备方法，其特征在于，采用模具进行加压烧结，模具为石墨热压模具，即石墨圆柱外桶内配有两个独立同轴的石墨圆柱体，下部的为石墨模具底托，上部的为石墨模具压盖；
多层复合陶瓷盘包括至少一个基础三明治结构，所述的一个基础三明治结构包括第一陶瓷层、第二陶瓷层以及位于第一陶瓷层和第二陶瓷层之间的金属电极层；制备方法具体包括以下步骤：
(1)用陶瓷粉体制备一个片状陶瓷素坯；把陶瓷素坯在低于烧结温度的预烧结温度下，进行预烧结，得到具有一定强度的预烧结陶瓷件；
(2)在预烧结陶瓷件的上表面上制备一金属电极层；
(3)将预烧结陶瓷件放入模具中石墨模具底托上，且覆有金属电极层的上表面朝上，在预烧结陶瓷件上表面提供一陶瓷前体层，沿着预烧结陶瓷件轴向方向在烧结温度下加压烧结成一体；其中，预烧结陶瓷件经加压烧结形成第二陶瓷层，陶瓷前体层经加压烧结形成第一陶瓷层，金属电极层位于所述第一陶瓷层和第二陶瓷层之间并与第一陶瓷层和第二陶瓷层形成一体化，即得到一个基础三明治结构；
步骤(3)所述陶瓷前体层为均匀分布的陶瓷粉体；步骤(1)所述预烧结陶瓷件的预烧结温度比步骤(3)烧结温度低100℃-400℃；步骤(3)所述的烧结温度为致密化烧结温度。
2.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，所述复合陶瓷盘包括两个基础三明治结构，其中第二陶瓷层的下表面还成型有一个金属电极层和一个第一陶瓷层，共形成两个基础三明治结构五层复合陶瓷盘，五层结构依次为第一陶瓷层/金属电极层/第二陶瓷层/金属电极层/第一陶瓷层；其制备方法包括以下步骤：
(1)用陶瓷粉体制备一个片状陶瓷素坯；把陶瓷素坯在低于烧结温度的预烧结温度下，进行预烧结，得到具有一定强度的预烧结陶瓷件；
(2)在预烧结陶瓷件的上表面和下表面分别制备一金属电极层，得到带有双金属电极层的预烧结陶瓷件；
(3)将陶瓷前体层、带有双金属电极层的预烧结陶瓷件依次按照如下的上下层关系：陶瓷前体层/带有双金属电极层预烧结陶瓷件/陶瓷前体层同轴配备到模具中石墨模具底托上，然后沿着预烧结陶瓷件轴向方向在烧结温度下加压烧结成一体；其中，预烧结陶瓷件经加压烧结形成第二陶瓷层，陶瓷前体层经加压烧结形成第一陶瓷层；所述两个基础三明治结构五层复合陶瓷盘制备中的两个陶瓷前体层相同或不同，对应的第一陶瓷层材料相同或不同；
步骤(3)所述陶瓷前体层为均匀分布的陶瓷粉体；步骤(1)所述预烧结陶瓷件的预烧结温度比步骤(3)烧结温度低100℃-400℃；步骤(3)所述的烧结温度为致密化烧结温度。
3.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，
步骤(1)所述预烧结陶瓷件，可耐水浸泡，并能够进行尺寸公差精度在0.03mm以内的车、铣、磨的精加工；步骤(1)所述片状陶瓷素坯的成型方法是等静压成型。
4.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，
还包括在步骤(2)在预烧结陶瓷件的上表面上制备一金属电极层之前，对所述的预烧结陶瓷件进行精加工，使其平面度更好、厚度更均匀，将预烧结陶瓷件加工至平面度不大于0.03mm。
5.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，
步骤(2)所述金属电极层通过丝网印刷工艺或者镀膜工艺成型到预烧结陶瓷件上；所述金属电极层的平面度不大于0.03mm。
6.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，
步骤(1)陶瓷粉体和步骤(3)所述陶瓷前体层的材料成分均选自氧化物、非氧化物中的一种或几种，其中氧化物选自氧化铝、氧化锆、镁铝尖晶石中的一种或两种，非氧化物选自氮化铝、氮化硅、碳化硅中的一种或两种；烧结之后第二陶瓷层和第一陶瓷层对应的为氧化物陶瓷、非氧化物陶瓷中的一种或几种，其中氧化物陶瓷选自氧化铝陶瓷、氧化锆陶瓷、镁铝尖晶石中的一种或两种，非氧化物陶瓷选自氮化铝、氮化硅、碳化硅中的一种或两种。
7.按照权利要求1所述的一种多层复合陶瓷盘的制备方法，其特征在于，
所述第一陶瓷层和第二陶瓷层的面积大于所述金属电极层的面积，金属电极层包覆在第一陶瓷层和第二陶瓷层之间，第一陶瓷层和第二陶瓷层外缘部分互相接触并经加压烧结成一体。
8.按照权利要求1-7任一项所述的方法制备得到的多层复合陶瓷盘。
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