CN105647106B - 一种中空陶瓷微珠peek复合覆铜板及其制备方法 - Google Patents

一种中空陶瓷微珠peek复合覆铜板及其制备方法 Download PDF

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CN105647106B
CN105647106B CN201610059934.1A CN201610059934A CN105647106B CN 105647106 B CN105647106 B CN 105647106B CN 201610059934 A CN201610059934 A CN 201610059934A CN 105647106 B CN105647106 B CN 105647106B
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段辉
王海宁
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Zibo Maiterui Engineering Material Co Ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B32B37/1018—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure using only vacuum
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

本发明公开了一种中空陶瓷微珠PEEK复合覆铜板，包括下述重量份数的原料：陶瓷微珠：0～50重量份；偶联剂：0～5重量份；PEEK：50～100重量份。本发明还公开了复合覆铜板的制备方法，包括如下步骤：(1)混炼成型：偶联剂活化处理陶瓷微珠，然后加入PEEK在温度320～400℃下混炼成型；(2)热层压合：步骤(1)混炼成型的材料压合铜箔，在90Kpa的真空条件下，于温度350～380℃，压力15～20Mpa，电加热层压机中保压3～6h。本发明的优点是：本发明目的在于提供一种中空陶瓷微珠PEEK复合覆铜板的制作方法，其制成的复合覆铜板具有极低的介电常数(～1.34)、低介质损耗，极高的耐热性等优点，拉伸强度和吸水率仅略有下降。

Description

一种中空陶瓷微珠PEEK复合覆铜板及其制备方法
技术领域
本发明属于高分子材料技术领域，尤其涉及一种中空陶瓷微珠PEEK复合覆铜板及其制备方法。
背景技术
聚醚醚酮(PEEK)树脂是一种性能优异的特种工程塑料，与其他特种工程塑料相比具有诸多显著优势，耐高温、机械性能优异、自润滑性好、耐化学品腐蚀、阻燃、耐剥离性、耐辐照性、绝缘性稳定、耐水解和易加工等，在航空航天、汽车制造、电子电气、医疗和食品加工等领域得到应用。也被应用于高频的基板材料，尤其是地面微波视讯、卫星通信、移动手机、军工雷达、航天航空、导弹导航等领域，但PEEK材料价格昂贵。阻碍了其广泛使用。虽然有学者研究了中空玻璃微珠在聚四氟乙烯(PTFE)等材料中的应用，但缺乏中空陶瓷微珠在成型工艺和性能极具特点的PEEK材料中的应用工艺研究。
发明内容
为了解决上述问题，本发明采用的技术方案为：
一种中空陶瓷微珠PEEK复合覆铜板，包括下述重量份数的原料：陶瓷微珠：0～50重量份；偶联剂：0～5重量份；PEEK：50～100重量份。偶联剂为硅烷偶联剂、钛酸酯偶联剂或二者的混合。
利用空心陶瓷微珠介电常数小、刚性大、热膨胀系数小等特点，将空心陶瓷微珠与PEEK共混，制备高频微波复合介电材料，可提高高频微波复合介电材料的电学和力学性能，同时，显著降低材料的成本(最大可降低40％)。
空心陶瓷微珠主要成分为TiO2、SiO2和Al2O3等，粒径：0.1～100μm。
一种中空陶瓷微珠PEEK复合覆铜板制备方法，包括如下步骤：
(1)混炼成型：偶联剂活化处理陶瓷微珠，然后加入PEEK在温度320～400℃下混炼成型；
(2)热层压合：步骤(1)混炼成型的材料压合铜箔，在90Kpa的真空条件下，于温度350～380℃，压力15～20Mpa，电加热层压机中保压3～6h。所述铜箔是厚度是0.01～0.05mm。
得到的中空陶瓷微珠PEEK复合覆铜板，介电常数1.34～3.15、耗散因子0.0011～0.007。
本发明优点是：得到的复合覆铜板
①极低的介电常数，最小可达1.34；
②极低的介质损耗率；
③良好的力学性能；
④显著降低成本。
具体实施方式
实施例1：用0.5重量份的硅烷偶联剂活化处理10重量份的陶瓷微珠，然后，与90重量份的PEEK在320℃下混炼成型。在90Kpa的真空条件下，于温380℃，15Mpa下电加热层压机中保压6小时热层压合铜箔。层压板材料的介电常数3.15、耗散因子0.007。
实施例2：用1.0重量份的钛酸酯偶联剂活化处理20重量份的陶瓷微珠，然后，与80重量份的PEEK在340℃下混炼成型。在90Kpa的真空条件下，于温度370℃，15Mpa下电加热层压机中保压5小时热层压合铜箔，铜箔厚0.01mm。层压板材料的介电常数2.7、耗散因子0.0035。
实施例3：用1.5重量份的硅烷偶联剂活化处理30重量份的陶瓷微珠，然后，与70重量份的PEEK在360℃下混炼成型。在90Kpa的真空条件下，于温度360℃，16Mpa下电加热层压机中保压5小时热层压合铜箔，铜箔厚0.05mm。层压板材料的介电常数2.3、耗散因子0.0026。
实施例4：用0.5重量份的硅烷偶联剂和0.5重量份的钛酸酯偶联剂活化处理20重量份的陶瓷微珠，然后，与80重量份的PEEK在370℃下混炼成型。在90Kpa的真空条件下，于温度350℃，17Mpa下电加热层压机中保压4小时热层压合铜箔，铜箔厚0.02mm。层压板材料的介电常数2.8、耗散因子0.0035。
实施例5：用0.5重量份的硅烷偶联剂和1.0重量份的钛酸酯偶联剂活化处理30重量份的陶瓷微珠，然后，与70重量份的PEEK在380℃下混炼成型。在90Kpa的真空条件下，于温度365℃，18Mpa下电加热层压机中保压3小时热层压合铜箔。层压板材料的介电常数2.35、耗散因子0.0027。
实施例6：用0.5重量份的硅烷偶联剂和1.0重量份的钛酸酯偶联剂活化处理40重量份的陶瓷微珠，然后，与60重量份的PEEK在390℃下混炼成型。在90Kpa的真空条件下，于温度375℃，19Mpa下电加热层压机中保压4小时热层压合铜箔。层压板材料的介电常数1.85、耗散因子0.0021。
实施例7：用1.5重量份的钛酸酯偶联剂活化处理40重量份的陶瓷微珠，然后，与70重量份的PEEK在400℃下混炼成型。在90Kpa的真空条件下，于温度375℃，20Mpa下电加热层压机中保压5小时热层压合铜箔，铜箔厚0.03mm。层压板材料的介电常数1.80、耗散因子0.002。
实施例8：用0.5重量份的硅烷偶联剂和1.0重量份的钛酸酯偶联剂活化处理50重量份的陶瓷微珠，然后，与50重量份的PEEK在400℃下混炼成型。在90Kpa的真空条件下，于温度380℃，20Mpa下电加热层压机中保压6小时热层压合铜箔，铜箔厚0.04mm。层压板材料的介电常数1.35、耗散因子0.0013。
实施例9：用1.5重量份的硅烷偶联剂活化处理50重量份的陶瓷微珠，然后，与50重量份的PEEK在400℃下混炼成型。在90Kpa的真空条件下，于温度380℃，20Mpa下电加热层压机中保压6小时热层压合铜箔。层压板材料的介电常数1.34、耗散因子0.0011。
实施例10：用2.5重量份的硅烷偶联剂和2.5重量份的钛酸酯偶联剂活化处理50重量份的陶瓷微珠，然后，与50重量份的PEEK在400℃下混炼成型。在90Kpa的真空条件下，于温度380℃，20Mpa下电加热层压机中保压6小时热层压合铜箔，铜箔厚0.04mm。层压板材料的介电常数1.35、耗散因子0.0013。

Claims (2)

1.一种中空陶瓷微珠PEEK复合覆铜板，其特征在于，用0.5重量份的硅烷偶联剂和1.0重量份的钛酸酯偶联剂活化处理50重量份的陶瓷微珠，然后，与50重量份的PEEK在400℃下混炼成型，在90Kpa的真空条件下，于温度380℃，20Mpa下电加热层压机中保压6小时热层压合铜箔，铜箔厚0.04mm，层压板材料的介电常数1.35、耗散因子0.0013。
2.一种中空陶瓷微珠PEEK复合覆铜板，其特征在于，用1.5重量份的硅烷偶联剂活化处理50重量份的陶瓷微珠，然后，与50重量份的PEEK在400℃下混炼成型，在90Kpa的真空条件下，于温度380℃，20Mpa下电加热层压机中保压6小时热层压合铜箔，层压板材料的介电常数1.34、耗散因子0.0011。
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