CN114805769B - 一种液晶聚酯和一种液晶聚酯复合材料和应用 - Google Patents
一种液晶聚酯和一种液晶聚酯复合材料和应用 Download PDFInfo
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- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical group C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 claims abstract description 10
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- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
- C08G63/605—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds the hydroxy and carboxylic groups being bound to aromatic rings
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Abstract
一种液晶聚酯复合材料,按重量份计,包括以下组分:液晶聚酯70份;激光成型添加剂2‑12份;所述的液晶聚酯,按液晶聚酯链段的摩尔百分含量计,包括以下重复单元:对羟基苯甲酸单元0.5‑30mol%、2‑羟基‑6‑萘甲酸单元30‑55mol%、联苯二酚单元20‑25mol%、对苯二甲酸单元20‑25mol%;所述的激光成型添加剂的平均粒径为5‑25微米。本发明通过在特定结构的液晶聚酯中添加特定平均粒径范围的激光成型添加剂,实现了激光成型添加剂的均匀分布,不仅能够提升液晶聚酯复合材料的镭雕化镀性能,并且具有低介电损耗的优点。
Description
技术领域
本发明涉及高分子材料技术领域,特别是涉及一种液晶聚酯复合材料及其制备方法和应用。
背景技术
激光直接成型(Laser Direct Structuring,LDS)或镭雕化镀性是指利用计算机控制激光束,将激光束照射到制件上,被激光束照射过的区域具有活化能力,该制件上具有活化能力的区域可以在化学镀液中沉积铜、镍、金等金属,没有被激光束照射过的区域则不能沉积铜、镍、金等金属,从而使这种树脂组合物在沉积金属时具有选择性。相对其它传统工艺,LDS技术可以在塑料基材上制作三维电路,设计自由度更大,从而节省空间,满足器件轻量化和小型化需求;同时,LDS技术精确度高,最小导线宽度可达150μm,最小线间宽度可达10μm。因此,基于LDS技术开发的LDS材料已经广泛应用于智能手机天线、笔记本电脑天线,医疗设备传感器、汽车设备传感器、电子电气等产品中。
随着5G信息时代的到来,信号峰值理论传输速度可达每秒数10Gb,具有低延迟、低损失、高传输的特性。更重要的是,电磁波频率越高,则波长越短,绕射能力就越差,传播过程中的电磁波的衰减也越大。因此,为了实现5G信号传输低损失特性,应用于5G领域的天线材料必须具有低介电损耗的特性。
但是,基于LDS技术开发的LCP-LDS材料因为激光成型添加剂(铜、镍、金等金属)的加入导致材料的介电损耗较高。目前市售的LCP-LDS材料在2.5GHz的介电损耗均≥0.005,而在5G领域中使用的天线材料一般要求介电损耗≤0.004(最好低于0.003),因此常规的LCP-LDS材料难以满足使用要求。这是由于激光敏感添加剂都为金属盐,当其分散不均匀时容易导致介电损耗的明显提升,而由于低粒径的金属氧化物易发生团聚现象,因此现有技术的一般分散方法很难实现激光成型添加剂的均匀分散,往往需要额外添加流动改性剂,造成成本的上升。CN201911038693.2公开了LCP液晶聚合物中常用的激光成型添加剂为镉、锌、铜、钴、镁、锡、钛、铁、铝、镍、金、银、钯、锰或铬的氧化物、磷酸氢氧盐、磷酸盐、硫酸盐或硫氰酸盐中一种或者至少两种等。但是,实际上,该专利仅关注了介电常数,并没有关注介电损耗性。
发明内容
本发明的目的在于,解决上述技术缺陷,提供一种液晶聚酯以及一种具有低介电损耗的优点的液晶聚酯复合材料,并且具有镭雕化镀性能好的优点。
本发明的另一目的在于提供上述液晶聚酯复合材料的应用。
本发明是通过以下技术方案实现的:
一种液晶聚酯,按液晶聚酯链段的摩尔百分比计,包括以下重复单元:对羟基苯甲酸单元0.5-30mol%、2-羟基-6-萘甲酸单元30-55mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%。
优选的,按液晶聚酯链段的摩尔百分比计,包括以下重复单元:对羟基苯甲酸单元1.5-2.5mol%、2-羟基-6-萘甲酸单元51-54mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%。
所述的液晶聚酯在高于其熔融温度20℃,1000s-1剪切速率下参照GB T 25278-2010标准,通过毛细管流变仪测定的熔融粘度为10~100Pa .s。
液晶聚酯的制备方法为:在反应釜中加入对羟基苯甲酸、2-羟基-6-萘甲酸、联苯二酚、对苯二甲酸。置换氮气后,在氮气氛下将反应温度升高到140-150℃回流反应2-4小时;之后以50-70℃/小时速率升温至310-330℃,保持在该温度下反应0.5-1小时后,抽真空至150-250Pa继续反应至搅拌功率达到预定值;然后将反应釜内加入氮气至压力为0.15-0.25MPa,通过釜底阀门排出,过水槽后用切粒机切成预聚物颗粒;将上述预聚物颗粒加入带有搅拌器的反应器中,然后在240-260℃,真空度为20-30Pa条件下固相缩聚反应4-6小时得到最终的液晶聚合物树脂。
一种液晶聚酯复合材料,按重量份计,包括以下组分:
液晶聚酯 70份;
激光成型添加剂 2-12份;
所述的液晶聚酯,按液晶聚酯链段的摩尔百分比计,包括以下重复单元:对羟基苯甲酸单元0.5-30mol%、2-羟基-6-萘甲酸单元30-55mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%;
所述的激光成型添加剂的平均粒径为5-25微米。
优选的,按液晶聚酯链段的摩尔百分比计,包括以下重复单元:对羟基苯甲酸单元1.5-2.5mol%、2-羟基-6-萘甲酸单元51-54mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%。
所述的液晶聚酯在高于其熔融温度20℃,1000s-1剪切速率下通过毛细管流变仪测定的熔融粘度为10~100Pa.s。
可选的,所述的激光成型添加剂选自镉、锌、铜、钴、镁、锡、钛、铁、铝、镍、金、银、钯、锰或铬的氧化物、磷酸氢氧盐、磷酸盐、硫酸盐或硫氰酸盐中的至少一种。
优选的,所述的激光成型添加剂的平均粒径为10-20微米。
可以根据实际需求决定是否加入0-50份增强填料;所述的增强填料选自玻璃纤维、磨碎玻璃纤维、硅灰石、无机矿物、云母粉、滑石粉、高岭土、玻璃薄片、二氧化硅、氧化钛、碳酸钙中的至少一种。
本发明得到的所述的液晶聚酯复合材料在2.5GHz的介电损耗小于等于0.003。
本发明的液晶聚酯复合材料的制备方法,包括以下步骤:按照配比,将各组分混合均匀,经过双螺杆挤出机挤出造粒,螺筒温度范围是290-350℃、螺杆转速为200-500rpm,得到液晶聚酯复合材料。
本发明的液晶聚酯复合材料的应用,用于制备5G天线材料。
本发明具有如下有益效果:
激光成型添加剂为金属盐,这些金属盐本身的的介电损耗值非常高,添加到液晶聚酯中会严重提升液晶聚酯复合材料的介电损耗值。如果激光成型添加剂的粒径过小(小于5微米),由于金属盐自身容易团聚,反而无法均匀分散;如果激光成型添加剂的粒径过大(大于25微米),一方面降低镭雕化镀性、另一方面介电损耗值高。对此,本发明设计了一种特殊链段结构的液晶聚酯,该液晶聚酯具有良好的流动性,特别是相对于其他链段结构的液晶聚酯具有对于金属盐更好的分散性,能够实现激光成型添加剂(金属盐)的均匀分散。进一步通过针对激光成型添加剂的粒径进行筛选,能够实现在保持良好镭雕化镀性的前提下降低介电损耗。使得本发明的介电损耗小于等于0.003(2.5GHz)。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
本发明所用原材料来源如下:
树脂名称 | 对羟基苯甲酸,mol% | 2-羟基-6-萘甲酸,mol% | 联苯二酚,mol% | 对苯二甲酸,mol% | 熔融粘度,Pa .s |
液晶聚酯A | 2 | 53 | 22.5 | 22.5 | 13.2 |
液晶聚酯B | 1.5 | 54 | 22.25 | 22.25 | 16.2 |
液晶聚酯C | 2.5 | 51 | 23.25 | 23.25 | 11.2 |
液晶聚酯D | 0.5 | 50.5 | 24.5 | 24.5 | 21.7 |
液晶聚酯E | 30 | 30 | 20 | 20 | 19.4 |
液晶聚酯F | 0.1 | 54.9 | 22.5 | 22.5 | 14.2 |
液晶聚酯G | 40 | 15 | 22.5 | 22.5 | 17.1 |
液晶聚酯H | 2.5 | 60.5 | 18.5 | 18.5 | 26.7 |
液晶聚酯I | 4 | 40 | 28 | 28 | 18.8 |
以上液晶聚酯的制备方法为:在配有氮气入口、带搅拌功率显示的搅拌器的250升反应釜中,加入对羟基苯甲酸、2-羟基-6-萘甲酸、联苯二酚、对苯二甲酸(TPA)。置换氮气后,在氮气氛下将反应温度升高到145℃回流反应3小时;之后以60℃/小时速率升温至320℃,保持在该温度下反应30分钟后,在30min内抽真空至200Pa继续反应至搅拌功率达到预定值;然后将反应釜内加入氮气至压力为0 .2MPa,通过釜底阀门排出,过水槽后用切粒机切成预聚物颗粒;将10kg上述预聚物颗粒加入50升带有搅拌器的反应器中,然后在250℃,真空度为25Pa条件下固相缩聚反应5小时得到最终的液晶聚合物树脂。
液晶聚酯J:XYDAR SRT-900 LOWMV, 熔融粘度20 Pa .s,索尔维公司。
液晶聚酯K:VECTRA® A950,熔融粘度18 Pa .s,塞拉尼斯公司。
激光成型添加剂A:铜-铬氧化物,平均粒径5.3微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂B:铜-铬氧化物,平均粒径10.0微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂C:铜-铬氧化物,平均粒径19.7微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂D:铜-铬氧化物,平均粒径24.6微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂E:铜-铬氧化物,平均粒径1.3微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂F:铜-铬氧化物,平均粒径30.4微米,质量配比氧化铜/氧化铬:1/1,自制。
激光成型添加剂G:锡-锑掺杂化合物,平均粒径5.3微米,质量配比磷酸亚锡/氧化锑:2/1,自制。
激光成型添加剂H:锰-亚铜掺杂化合物,平均粒径8.7微米,质量配比磷酸二氢锰/硫酸亚铜:1/2,自制。
激光成型添加剂I:钨-锑氧化物,平均粒径6.2微米,质量配比氧化钨/氧化锑:1/1,自制。
以上激光成型添加剂的制备方法为:将铜-铬氧化物、锰-亚铜掺杂化合物钨-锑氧化物的原料按照各组分的原料配比称量物料,湿磨,将磨好的物料烘干去除水分,然后粉碎,将粉碎后的粉体放入高温炉中升温到1000-1500℃煅烧0.5-3hrs,通过筛选后得到目标产物。
玻璃纤维:市售,平行实验中采用同种玻纤。
实施例和对比例液晶聚酯复合材料的制备方法:按照配比,将各组分混合均匀,经过双螺杆挤出机挤出造粒,螺筒温度范围是290-320-350-320-290-290-290-290-290-290-320-350℃、螺杆转速为200-500rpm,得到液晶聚酯复合材料。
各项测试方法:
(1)镀层厚度:将液晶聚酯复合材料在290~350℃的条件下进行加热熔融、注射成型,制作成100mm×100mm×2mm的平板状试验片,经镭雕化镀之后,使用影像量测仪测试沉积的金属镀层厚度,设计镀层厚度为10微米,实测镀层厚度越接近10微米越好。
(2)百格测试:参照GB/T9286-1998,用百格刀在镭雕化镀后测试样本表面划10×10个(100个)1mm×1mm小网格,用毛刷将测试区域的碎片刷干净;用3M600号胶纸或等同效力的胶纸牢牢粘住被测试小网格,并用橡皮擦压平整后,快速拉起胶带,观察脱落数量判断其镀层结合力,试验结果分级如下:
0级:切割边缘完全平滑,无一格脱落;
1级:在切口交叉处有少许镀层脱落,但交叉切割面积受影响不能明显大于5%;
2级:在切口交叉处和/或沿切口边缘有涂层脱落,受影响的交叉切割面积明显大于5%,但不能明显大于15%;
3级:镀层沿切口边缘部分或全部以大于碎片脱落,和/或在格子不同部位上部分或全部剥落,受影响的交叉切割面积明显大于15%,但不能明显大于35%;
4级:镀层沿切割边缘大碎片剥落,和/或一些方格部分或全部出现脱落,受影响的交叉切割面积明显大于35%,但不能明显大于65%;
5级:剥落的程度超过4级。
(3)介电损耗测试:将液晶聚合物复合材料在290~350℃的条件下进行加热熔融、注射成型,制作成100mm×100mm×2mm的平板状试验片,参照ASTM D150标准,利用分离介质谐振器法(SPDR法),来测定频率2.5GHz的介电损耗角正切。
表1:实施例1-7液晶聚酯复合材料组分(重量份)及测试结果
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | |
液晶聚酯A | 70 | 70 | 70 | ||||
液晶聚酯B | 70 | ||||||
液晶聚酯C | 70 | ||||||
液晶聚酯D | 70 | ||||||
液晶聚酯E | 70 | ||||||
激光成型添加剂A | 8 | 8 | 8 | 8 | 8 | 2 | 12 |
玻璃纤维 | 25 | 25 | 25 | 25 | 25 | 0 | 50 |
镀层厚度,微米 | 10.05 | 9.97 | 10.02 | 10.11 | 9.93 | 10.04 | 9.96 |
百格测试,级 | 0 | 0 | 0 | 0 | 0 | 1 | 0 |
介电损耗(2.5GHz) | 0.0016 | 0.0018 | 0.0020 | 0.0025 | 0.0028 | 0.0012 | 0.0027 |
由实施例1-5可知,优选重复单元构成的液晶聚酯具有更低的介电损耗、镀层厚度也更精确。
由实施例6-7可知,激光成型添加剂的添加量显著影响介电损耗,在本发明的添加量下能够控制介电损耗低于0.003。
表2:实施例8-13液晶聚酯复合材料组分(重量份)及测试结果
实施例8 | 实施例9 | 实施例10 | 实施例11 | 实施例12 | 实施例13 | |
液晶聚酯A | 70 | 70 | 70 | 70 | 70 | 70 |
激光成型添加剂B | 8 | |||||
激光成型添加剂C | 8 | |||||
激光成型添加剂D | 8 | |||||
激光成型添加剂G | 8 | |||||
激光成型添加剂H | 8 | |||||
激光成型添加剂I | 8 | |||||
玻璃纤维 | 25 | 25 | 25 | 25 | 25 | 25 |
镀层厚度,微米 | 10.01 | 10.00 | 10.04 | 10.06 | 9.95 | 10.06 |
百格测试,级 | 0 | 0 | 1 | 0 | 0 | 1 |
介电损耗(2.5GHz) | 0.0010 | 0.0012 | 0.0023 | 0.0018 | 0.0018 | 0.0019 |
由实施例1/8-13可知,优选的激光成型添加剂平均粒径下,镀层厚度更精确,并且介电损耗更低。
表2:对比例液晶聚酯复合材料组分(重量份)及测试结果
对比例1 | 对比例2 | 对比例3 | 对比例4 | 对比例5 | 对比例6 | 对比例7 | 对比例8 | |
液晶聚酯A | 70 | 70 | ||||||
液晶聚酯F | 70 | |||||||
液晶聚酯G | 70 | |||||||
液晶聚酯H | 70 | |||||||
液晶聚酯I | 70 | |||||||
液晶聚酯J | 70 | |||||||
液晶聚酯K | 70 | |||||||
激光成型添加剂A | 8 | 8 | 8 | 8 | 8 | 8 | ||
激光成型添加剂E | 8 | |||||||
激光成型添加剂F | 8 | |||||||
玻璃纤维 | 25 | 25 | 25 | 25 | 25 | 25 | 25 | 25 |
镀层厚度,微米 | 9.91 | 10.14 | 10.08 | 9.76 | 10.10 | 9.93 | 10.10 | 10.09 |
百格测试,级 | 0 | 0 | 0 | 0 | 0 | 0 | 2 | 1 |
介电损耗(2.5GHz) | 0.0053 | 0.0048 | 0.0045 | 0.0039 | 0.0041 | 0.0050 | 0.0038 | 0.0042 |
由实施例与对比例1-4可知,本发明的液晶聚酯适用于激光成型制造,并且具有低介电损耗的优点。
由对比例5/6可知,现有技术常用于激光成型的液晶聚酯虽然具有很好的激光成型制造性,但是介电损耗高。
由对比例7/8可知,激光成型添加剂的平均粒径显著影响液晶聚酯复合材料的介电损耗,当其平均粒径过高或过低时,无法实现介电损耗低于0.003。
Claims (9)
1.一种液晶聚酯复合材料,其特征在于,按重量份计,包括以下组分:
液晶聚酯 70份;
激光成型添加剂 2-12份;
所述的液晶聚酯,按液晶聚酯链段的摩尔百分比计,由以下重复单元构成:对羟基苯甲酸单元0.5-30mol%、2-羟基-6-萘甲酸单元30-55mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%;
所述的激光成型添加剂的平均粒径为5-25微米。
2.根据权利要求1所述的液晶聚酯复合材料,其特征在于,所述的液晶聚酯,按液晶聚酯链段的摩尔百分含量计,由以下重复单元构成:对羟基苯甲酸单元1.5-2.5mol%、2-羟基-6-萘甲酸单元51-54mol%、联苯二酚单元20-25mol%、对苯二甲酸单元20-25mol%。
3. 根据权利要求1或2所述的液晶聚酯复合材料,其特征在于,所述的液晶聚酯在高于其熔融温度20℃,1000s-1剪切速率下参照GB T 25278-2010标准,通过毛细管流变仪测定的熔融粘度为10~100Pa .s。
4.根据权利要求1所述的液晶聚酯复合材料,其特征在于,所述的激光成型添加剂选自镉、锌、铜、钴、镁、锡、钛、铁、铝、镍、金、银、钯、锰或铬的氧化物、磷酸氢氧盐、磷酸盐、硫酸盐或硫氰酸盐中的至少一种。
5.根据权利要求1所述的液晶聚酯复合材料,其特征在于,所述的激光成型添加剂的平均粒径为10-20微米。
6.根据权利要求1所述的液晶聚酯复合材料,其特征在于,按重量份计,还包括0-50份增强填料;所述的增强填料选自无机矿物。
7.根据权利要求1所述的液晶聚酯复合材料,其特征在于,按重量份计,还包括0-50份增强填料;所述的增强填料选自玻璃纤维、硅灰石、云母粉、滑石粉、高岭土、玻璃薄片、二氧化硅、氧化钛、碳酸钙中的至少一种。
8.根据权利要求1-7任一项所述的液晶聚酯复合材料,其特征在于,所述的液晶聚酯复合材料在2.5GHz的介电损耗小于等于0.003。
9.权利要求1-8任一项所述的液晶聚酯复合材料的应用,其特征在于,用于制备5G天线材料。
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