CN107933031A - 一种复合型高介电材料的制备方法 - Google Patents

一种复合型高介电材料的制备方法 Download PDF

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CN107933031A
CN107933031A CN201711166525.2A CN201711166525A CN107933031A CN 107933031 A CN107933031 A CN 107933031A CN 201711166525 A CN201711166525 A CN 201711166525A CN 107933031 A CN107933031 A CN 107933031A
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邹黎清
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SUZHOU KEMAO ELECTRONIC MATERIAL TECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/28Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/285Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/045Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J2371/00Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2371/02Polyalkylene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals

Abstract

本发明公开了一种复合型高介电材料的制备方法,称取V2O5、Li2O和MgO加入球磨机中,并加入聚丙二醇二甲基丙烯酸酯混合研磨,得到混合料A;随后放入模具中热压成型得料B;将料B加入水溶液中,于温度35‑45℃下超声分散10‑20min,制得悬浮液;用浸渍提拉法在基底表面制得均匀薄膜,干燥后得到第一层;将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到氧化石墨烯悬浮液;用浸渍提拉法在第一层表面制得60‑90nm厚度的均匀薄膜,干燥后得到第二层;重复以上步骤多次,即可得到所述复合型高介电材料。

Description

一种复合型高介电材料的制备方法
技术领域
[0001] 本发明属于电子材料领域,特别涉及一种复合型高介电材料的制备方法。
背景技术
[0002] 介电材料是可用于控制存储电荷及电能的绝缘材料,在现代电子及电力系统中具 有重要的战略地位。为了要满足电子产品高功能化、高速高频的需求,必需增加电子构装基 板上的主动组件及被动组件。这使得电路板面积增加且成本提高。为了达到轻薄短小的需 求,势必引起电路与组件密度增加,造成电磁干扰与噪声增加且降低可靠度。为了解决这一 问题,需要改良被动组件,例如电容的整合。为了达到上述目的,兼具高分子的机械性质与 高介电性质的高分子-无机复合材料是这种电容材料的最佳选择。
[0003] 为了增加埋入式电容介电材料的应用,如何提高复合材料的介电常数是目前这类 型材料开发的瓶颈与重点。单纯的无机材料虽具有高介电常数,但分散在环氧树脂中的粉 体由于偶极排列不规则,会使得电偶极偏极化的效应被抵销。仅通过添加高含量高介电常 数的粉体来提供复合材料的介电常数值是相当有限的,而且添加量过高将使得基板的机械 性质降低。但导电粉体的增加还将同时增加材料系统的介电常数而导致漏电流的增加,这 会降低材料的稳定性及可靠度,并限制其在电子产业的应用需求。
发明内容
[0004] 针对上述缺陷,本发明的目的是提供一种复合型高介电材料的制备方法,以氧化 石墨烯导电层-复合型聚合物绝缘层-导电层多次交替层状结构,进一步使材料的介电常数 高、介电损耗小,且朝性好。
[0005] 本发明的目的可以通过以下技术方案实现: 一种复合型高介电材料的制备方法,包括如下步骤: Sl:按质量比1:2-5:3称取V2〇5、Li2〇和MgO加入球磨机中,并加入固液比为1-5:10的聚 丙二醇二甲基丙烯酸酯后混合研磨20_40min,球料比为1-4:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为200-240°C,压 强18-22MPa,保压时间15-25min,得料B; S3:将料B加入水溶液中,于温度35-45°C下超声分散10_20min,制得45-65g/L的悬浮 液;用浸渍提拉法在基底表面制得1.2-2.5μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度2-5g/L的氧化石墨烯 悬浮液;用浸渍提拉法在第一层表面制得60_90nm厚度的均匀薄膜,干燥后得到第二层;重 复步骤S3-S4次数5-10次,即可得到所述复合型高介电材料。
[0006] 优选的,步骤Sl中所述V2O5、Li2〇和MgO的质量比为1:4:3; V2〇5/Li2〇/MgO混合物和 聚丙二醇二甲基丙烯酸酯的固液比为3:10;混合研磨35min,球料比为2:1。
[0007] 优选的,步骤S2中所述热压的温度为220°C,压强20MPa,保压时间23min。
[0008] 优选的,步骤S3中所述温度42°C下超声分散18min,制得58g/L的悬浮液。
[0009] 优选的,步骤S3中用浸渍提拉法在基底表面制得2.2μπι厚度的均匀薄膜。
[0010] 优选的,步骤S4中所述氧化石墨烯悬浮液的浓度3.5g/L;用浸渍提拉法在第一层 表面制得85nm厚度的均匀薄膜。
[0011] 优选的,步骤S4中所述重复步骤S3-S4的次数为8次。
[0012]根据上述任意一条所述所制备得到的复合型高介电材料。
[0013] 本发明与现有技术相比,其有益效果为: 本发明所述一种复合型高介电材料的制备方法,用聚丙二醇二甲基丙烯酸酯包裹 V205/Li20/Mg0混合料,并经热压、分散、浸渍提拉后制备成第一层;采用氧化石墨烯悬浮液 制备成第二层,第一层和第二层之间相互交替呈现,进而得到导电层-绝缘层彼此交替的介 电材料;优化两层薄膜的厚度关系使得最终得到的介电材料介电常数高、介电损耗小,且韧 性好。
具体实施方式
[0014] 以下结合实施例对本发明作进一步的说明。
[0015] 实施例1 Sl:按质量比1: 2: 3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为1:10的聚丙二 醇二甲基丙烯酸酯后混合研磨20min,球料比为1:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为200°C,压强 18MPa,保压时间15min,得料B; S3:将料B加入水溶液中,于温度35°C下超声分散IOmin,制得45g/L的悬浮液;用浸渍提 拉法在基底表面制得1.2μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度2g/L的氧化石墨烯悬 浮液;用浸渍提拉法在第一层表面制得60nm厚度的均匀薄膜,干燥后得到第二层;重复步骤 S3-S4次数5次,即可得到所述复合型高介电材料。
[0016] 实施例2 SI:按质量比1:5: 3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为5:10的聚丙二 醇二甲基丙烯酸酯后混合研磨40min,球料比为4:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为240°C,压强 22MPa,保压时间25min,得料B; S3:将料B加入水溶液中,于温度45 °C下超声分散20min,制得65g/L的悬浮液;用浸渍提 拉法在基底表面制得2.5μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度5g/L的氧化石墨烯悬 浮液;用浸渍提拉法在第一层表面制得90nm厚度的均匀薄膜,干燥后得到第二层;重复步骤 S3-S4次数10次,即可得到所述复合型高介电材料。
[0017] 实施例3 SI:按质量比1:3: 3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为2:10的聚丙二 醇二甲基丙烯酸酯后混合研磨25min,球料比为2:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为220°C,压强 19MPa,保压时间18min,得料B; S3:将料B加入水溶液中,于温度40°C下超声分散12min,制得50g/L的悬浮液;用浸渍提 拉法在基底表面制得1.5μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度3g/L的氧化石墨烯悬 浮液;用浸渍提拉法在第一层表面制得65nm厚度的均匀薄膜,干燥后得到第二层;重复步骤 S3-S4次数7次,即可得到所述复合型高介电材料。
[0018] 实施例4 SI:按质量比1:4: 3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为4:10的聚丙二 醇二甲基丙烯酸酯后混合研磨35min,球料比为3:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为235°C,压强 20MPa,保压时间22min,得料B; S3:将料B加入水溶液中,于温度42°C下超声分散16min,制得60g/L的悬浮液;用浸渍提 拉法在基底表面制得2. Ομπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度4g/L的氧化石墨烯悬 浮液;用浸渍提拉法在第一层表面制得85nm厚度的均匀薄膜,干燥后得到第二层;重复步骤 S3-S4次数9次,即可得到所述复合型高介电材料。
[0019] 实施例5 SI:按质量比1:4: 3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为3:10的聚丙二 醇二甲基丙烯酸酯后混合研磨35min,球料比为2:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为220°C,压强 20MPa,保压时间23min,得料B; S3:将料B加入水溶液中,于温度42°C下超声分散18min,制得58g/L的悬浮液;用浸渍提 拉法在基底表面制得2.2μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度3.5g/L的氧化石墨烯 悬浮液;用浸渍提拉法在第一层表面制得85nm厚度的均匀薄膜,干燥后得到第二层;重复步 骤S3-S4次数8次,即可得到所述复合型高介电材料。
[0020] 将上述新型高介电材料性能测试(25°C、10KHZ),结果如下:
Figure CN107933031AD00051
本发明不限于这里的实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴 所做出的改进和修改都应该在本发明的保护范围之内。

Claims (8)

1. 一种复合型高介电材料的制备方法,其特征在于,包括如下步骤: SI:按质量比1:2-5:3称取V2〇5、Li20和MgO加入球磨机中,并加入固液比为1-5:10的聚 丙二醇二甲基丙烯酸酯后混合研磨20_40min,球料比为1-4:1,得到混合料A; S2:将步骤Sl中所述混合料A放入模具中热压成型,其中,热压的温度为200-240°C,压 强18-22MPa,保压时间15-25min,得料B; S3:将料B加入水溶液中,于温度35-45°C下超声分散10_20min,制得45-65g/L的悬浮 液;用浸渍提拉法在基底表面制得1.2-2.5μπι厚度的均匀薄膜,干燥后得到第一层; S4:将氧化石墨烯粉末加入无水乙醇中,超声分散均匀,得到浓度2-5g/L的氧化石墨烯 悬浮液;用浸渍提拉法在第一层表面制得60_90nm厚度的均匀薄膜,干燥后得到第二层;重 复步骤S3-S4次数5-10次,即可得到所述复合型高介电材料。
2. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤Sl中所 述V2O^Li2O和MgO的质量比为l:4:3;V205/Li20/Mg0混合物和聚丙二醇二甲基丙烯酸酯的固 液比为1:8;混合研磨35min,球料比为2:1。
3. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤S2中所 述热压的温度为220°C,压强20MPa,保压时间23min。
4. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤S3中所 述温度42 °C下超声分散18min,制得58g/L的悬浮液。
5. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤S3中用 浸渍提拉法在基底表面制得2.2μπι厚度的均匀薄膜。
6. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤S4中所 述氧化石墨烯悬浮液的浓度3.5g/L;用浸渍提拉法在第一层表面制得85nm厚度的均匀薄 膜。
7. 根据权利要求1所述的一种复合型高介电材料的制备方法,其特征在于,步骤S4中所 述重复步骤S3-S4的次数为8次。
8. 根据权利要求1 -7任意一条所述所制备的复合型高介电材料。
CN201711166525.2A 2017-11-21 2017-11-21 一种复合型高介电材料的制备方法 Pending CN107933031A (zh)

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CN1847194A (zh) * 2005-04-04 2006-10-18 Tdk株式会社 电子部件、电介质陶瓷组合物及其制造方法
CN101045630A (zh) * 2006-03-30 2007-10-03 华新科技股份有限公司 介电材料成份
CN103538312A (zh) * 2013-09-10 2014-01-29 浙江工业大学 一种交替层状氧化石墨烯/聚乙烯醇介电材料及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1847194A (zh) * 2005-04-04 2006-10-18 Tdk株式会社 电子部件、电介质陶瓷组合物及其制造方法
CN101045630A (zh) * 2006-03-30 2007-10-03 华新科技股份有限公司 介电材料成份
CN103538312A (zh) * 2013-09-10 2014-01-29 浙江工业大学 一种交替层状氧化石墨烯/聚乙烯醇介电材料及其制备方法

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