CN102260378B - 复合材料、用其制作的高频电路基板及其制作方法 - Google Patents

复合材料、用其制作的高频电路基板及其制作方法 Download PDF

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CN102260378B
CN102260378B CN2011101171723A CN201110117172A CN102260378B CN 102260378 B CN102260378 B CN 102260378B CN 2011101171723 A CN2011101171723 A CN 2011101171723A CN 201110117172 A CN201110117172 A CN 201110117172A CN 102260378 B CN102260378 B CN 102260378B
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circuit board
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Abstract

本发明提供一种复合材料、用其制作的高频电路基板及其制作方法,该复合材料包括:具有低介电损耗的氟聚合物分散乳液;多孔隙的膨胀聚四氟乙烯薄膜;及粉末填料。使用该复合材料制作的高频电路基板,包括:数张相互叠合的由所述复合材料制作的预浸料及分别压覆于其两侧的铜箔。本发明采用介电性能优异的多孔隙的ePTFE薄膜作为载体材料,能够降低复合材料及高频电路基板的介电常数和介质损耗角正切;且多孔隙的ePTFE薄膜平整度、均匀性好,用其作为载体材料,制作成的高频电路基板及预浸料具有介电常数在X、Y方向各向同性;该复合材料制作的预浸料厚度可以根据采用不同厚度的多孔隙的ePTFE薄膜的厚度调节,避免了现有技术中使用浇注法生产厚膜产生的裂纹问题。

Description

复合材料、用其制作的高频电路基板及其制作方法技术领域[0001] 本发明涉及复合材料技术领域,尤其涉及一种复合材料、用其制作的高频电路基板及其制作方法。背景技术[0002] 近年来,随着信息通讯设备高性能化、高功能化以及网络化的发展,为了高速传输及处理大容量信息,操作信号趋向于高频化,电子产品的使用频率持续走高,要求基板材料的介电常数越来越低,介电损耗越来越小,而且要求基板介电常数的均匀性要好。[0003]目前高频电路基板使用低介电常数的树脂来获得良好的高频性能,这些低介电常数的树脂包括有由聚苯醚、氰酸酯、含有碳-碳不饱和双键的只由碳氢元素构成的热固性树脂、PTFE等几种树脂。覆铜板一般使用玻璃纤维布作为增强材料。但是玻璃纤维布的介电常数最低只可以做到3. 7(Q玻璃),受玻璃纤维布介电常数大的影响,除PTFE外,其它树脂制作的覆铜板的介电常数很难降低。[0004] 另一方面,在目前高频电路基板中,因使用编织材料做增强材料(如玻璃纤维布), 编织纤维布因编织的原因以及编织纤维交叉部分的节点存在,使得电路板中的介电常数在平面的X、Y方向的不是各向同性,存在X、Y方向的介电常数差异。这样高频信号在高频电路基板中传输时,因在X、Y方向的介电常数的不同产生信号的衰减,影响信号传输的稳定性。[0005] 美国专利US6218015采用两种聚四氟乙烯树脂配合并混合填料浇铸成薄膜后进行电路基板的制作。这种方法制作的电路材料因整板采用热塑性聚四氟乙烯树脂,介电性能优异,X、Y方向的介电常数也不存在差异,但这种浇注方法制作较厚的薄膜时容易产生裂纹,成品率不高;特别是在需要制作厚度较大的电路板时,需要许多层薄膜叠加在一起制成,生产效率不高。[0006] 美国专利US4772509采用多孔隙的膨胀聚四氟乙烯薄膜浸溃聚酰亚胺制作成半固化片,然后进行电路基板的制作。美国专利US5652055采用多孔隙的膨胀聚四氟乙烯薄膜浸溃热固性树脂制作电路基板。但是这两个专利因采用介质损耗角正切大(介质损耗角正切大于O. 01)的热固性树脂进行电路基板的制作,其介电性能要比专利US6218015采用聚四氟乙烯树脂制作的电路基板介电性能差。发明内容[0007] 本发明的目的在于提供一种复合材料,采用多孔隙的ePTFE薄膜为载体材料,提供预浸料及高频电路基板介电常数在X、Y方向各向同性,能够降低高频电路基板的介电常数和介质损耗角正切。[0008] 本发明的另一目的在于提供使用上述复合材料制作的高频电路基板,具有介电常数在X、Y方向各向同性,及高频介电性能,在高频电路的信号传输中效果更好。[0009] 本发明的再一目的在于提供使用上述复合材料制作的高频电路基板的制作方法,采用多孔隙的ePTFE薄膜为载体材料,具有良好的成型性,不产生裂纹,工艺操作简便。[0010] 为实现上述目的,本发明提供一种复合材料,其组成物包括:[0011] (I)具有低介电损耗的氟聚合物分散乳液;[0012] (2)多孔隙的膨胀聚四氟乙烯薄膜(ePTFE薄膜);及[0013] (3)粉末填料。[0014] 所述具有低介电损耗的氟聚合物为聚四氟乙烯(PTFE)、四氟乙烯-全氟烷氧基乙烯基醚共聚物(PFA)、及全氟乙烯丙烯共聚物(FEP)中的一种或多种。[0015] 所述多孔隙的膨胀聚四氟乙烯薄膜由聚四氟乙烯树脂制成,该聚四氟乙烯树脂不添加或添加有陶瓷填料。[0016] 所述多孔隙的膨胀聚四氟乙烯薄膜是通过膨胀拉伸方法制作而成,其孔径为 Γ100 μ m,孔隙率为30〜98%,厚度为O. 5〜300 μ m。[0017] 所述粉末填料含量占具有低介电损耗的氟聚合物分散乳液和粉末填料总量的 (Γ70体积% ;粉末填料的粒径中度值为O. 01-15 μ m,最大粒径不超过100 μ m。[0018] 所述粉末填料选自结晶型二氧化硅、熔融型的二氧化硅、球型二氧化硅、氧化铝、 钛酸锶、钛酸钡、钛酸锶钡、氮化硼、氮化铝、碳化硅、二氧化钛、玻璃粉、玻璃短切纤维、滑石粉、云母粉、碳黑、碳纳米管、金属粉、及聚苯硫醚中的一种或多种。[0019] 还包括(4)助剂,该助剂包括有乳化剂及分散剂。[0020] 本发明还提供一种高频电路基板,包括:数张相互叠合的预浸料及分别压覆于其两侧的金属箔,该数张预浸料均由所述复合材料制作。所述金属箔,为铜、黄铜、铝、镍、或这些金属的合金或复合金属箔。[0021] 同时,本发明提供一种上述高频电路基板的制作方法,包括下述步骤:[0022] 步骤I、称取复合材料的组成物:(1)具有低介电损耗的氟聚合物分散乳液;(2)多孔隙的膨胀聚四氟乙烯薄膜;(3)粉末填料;[0023] 步骤2、将具有低介电损耗的氟聚合物分散乳液,用水稀释至适当的粘度,然后用氨水调节PH值至8-12,将粉末填料和助剂混合,加入到上述调节好的分散乳液中,搅拌混合,使粉末填料均一的分散在其中,制得胶液;[0024] 步骤3、用上述胶液浸溃多孔隙的膨胀聚四氟乙烯薄膜,并控制到合适的厚度,然后于8(T30(TC烘烤去除水分及助剂,形成预浸料;[0025] 步骤4、将上述的预浸料数张相叠合,上下各压覆一张金属箔,放进压机进行热压制得所述高频电路基板,热压温度为35(T400°C,热压压力为25〜100Kg/cm2。[0026] 所述胶液的固体含量为3(Γ80% ;所述胶液在多孔隙的膨胀聚四氟乙烯薄膜表面上形成氟聚合物树脂层,其厚度控制在20微米以下。[0027] 本发明的有益效果:首先,采用介电性能优异的多孔隙的ePTFE薄膜作为载体材料,能够降低复合材料及高频电路基板的介电常数和介质损耗角正切;[0028] 其次,多孔隙的ePTFE薄膜平整度、均匀性好,用其作为载体材料,制作成的高频电路基板及预浸料具有介电常数在X、Y方向各向同性;[0029] 再次,预浸料的厚度可以根据采用不同厚度的多孔隙的ePTFE薄膜的厚度调节, 避免了现有技术(如US6218015专利)中使用浇注法生产厚膜产生的裂纹问题。具体实施方式[0030] 本发明提供一种复合材料,包括:(1)具有低介电损耗的氟聚合物分散乳液;(2) 多孔隙的膨胀聚四氟乙烯薄膜(ePTFE薄膜);(3)粉末填料。[0031] 作为本发明的具有低介电损耗的氟聚合物分散乳液的实例,包括聚四氟乙烯,和含氟的共聚物等,可以列举的有聚四氟乙烯(PTFE)分散乳液、四氟乙烯一全氟烷氧基乙烯基醚共聚物(PFA)分散乳液、全氟乙烯丙烯共聚物(FEP)分散乳液,上述分散乳液可一种或多种混合使用。本发明所述的分散乳液是以水为介质,将259Γ60%的氟聚合物微粒分散在水里,通过非离子表面活性剂使之处于稳定分散状态,形成一种乳液。分散乳液中氟聚合物微粒粒径在O. 02、. 5微米范围内,以方便后面的浸溃。[0032] 本发明所述的多孔隙的ePTFE薄膜,这种薄膜可以是通过膨胀拉伸方法制作而成,在其中有大量的开口的孔隙,孔隙的大小以可方便树脂和填料进入为好。根据本发明, 所述的多孔隙的ePTFE薄膜选用孔径为f 100 μ m、孔隙率为30、8%、厚度O. 5^300 μ m的 ePTFE薄膜,优选孔径为3〜50 μ m、孔隙率为50〜98%、厚度30〜300 μ m的ePTFE薄膜。该ePTFE 薄膜因内部有大量孔隙存在,在浸溃时,可以方便分散乳液、粉末填料等材料的进入。[0033] 本发明所述的多孔隙的ePTFE薄膜,可以是纯PTFE树脂(聚四氟乙烯树脂)制成的,也可以是添加了陶瓷填料的PTFE树脂制成。根据本发明,所述的多孔隙的ePTFE薄膜表面以经过一定的处理为好,优选等离子体处理。[0034] 本发明的复合材料还可加入粉末填料,粉末填料起着改善尺寸稳定性、降低CTE 等目的。所述粉末填料的含量占具有低介电损耗的氟聚合物和粉末填料总量的(T70Vol% (体积百分比),优选3(T55Vol%。粉末填料包括有结晶型二氧化硅、熔融型的二氧化硅、球型二氧化硅、钛酸锶、钛酸钡、钛酸锶钡、氮化硼、氮化铝、碳化硅、氧化铝、二氧化钛、玻璃粉、 玻璃短切纤维、滑石粉、云母粉、碳黑、碳纳米管、金属粉、聚苯硫醚等,以上填料可以单独使用或混合使用,其中,最佳填料是熔融型的二氧化硅或二氧化钛。为方便填料可以进入到 ePTFE薄膜的孔隙中,填料的粒径中度值为O. 0Γ15 μ m,最大粒径不超过100 μ m,优选填料的粒径中度值为O. 5^10 μ m0为达到更好的性能,粉末填料的表面可以经过处理,如使用偶联剂进行处理等。还包括助剂,助剂包括有乳化剂及分散剂等。[0035] 使用上述复合材料制作高频电路基板的方法,包括下述步骤:[0036] 步骤I、称取复合材料的组成物:(1)具有低介电损耗的氟聚合物分散乳液;(2)多孔隙的膨胀聚四氟乙烯薄膜;(3)粉末填料。[0037] 步骤2、将具有低介电损耗的氟聚合物分散乳液,用水稀释至适当的粘度,然后用氨水调节PH值至8-12,将粉末填料和助剂混合,加入到上述调节好的分散乳液中,搅拌混合,使粉末填料均一的分散在其中,制得胶液;[0038] 步骤3、用上述胶液浸溃多孔隙的ePTFE薄膜,并控制到合适的厚度,然后在 8(T30(TC烘烤除去水分、助剂等形成预浸料。所述胶液在多孔隙的膨胀聚四氟乙烯薄膜表面上形成氟聚合物树脂层,预浸料的厚度通过多孔隙的ePTFE薄膜,以及多孔隙的ePTFE薄膜上的氟聚合物树脂层的厚度共同决定。为了获取不同厚度的预浸料,可以采用不同厚度的多孔隙的ePTFE薄膜,在浸溃由所述氟聚合物分散乳液等形成的胶液后,在胶液填充满 ePTFE薄膜孔隙后,控制ePTFE薄膜上的树脂层厚度在20微米以下,优选控制在10微米以下,这样可以保证制作更厚(大于250微米)的预浸料而避免多孔隙的ePTFE薄膜上浸溃的5氟聚合物树脂层产生裂纹。[0039] 所述多孔隙的ePTFE薄膜上的氟聚合物树脂层厚度通过氟聚合物分散乳液的树脂及填料的固体含量来控制。树脂混合物(即胶液)的固体含量可调节在3(Γ80%之间,优选 35〜50%。[0040] 浸溃操作可以采用覆铜板制作的通用浸溃上胶机进行,上胶机烘箱的温度可以分段设定,烘箱采用的温度范围为8(T300°C,以去除水分以及乳化剂、分散剂等。[0041] 步骤4、将上述的预浸料数张相叠合,上下各压覆一张金属箔,放进压机进行热压制得所述高频电路基板,热压温度为35(T400°C,热压压力为25〜100Kg/cm2。所述金属箔, 为铜、黄铜、铝、镍、或这些金属的合金或复合金属箔。[0042] 所制作的高频电路基板,包括:数张相互叠合的预浸料及分别压覆于其两侧的金属箔,该数张预浸料均由所述复合材料制作。[0043] 针对上述制成的高频电路基板的介电性能,即介电常数和介质损耗角正切、高频性能及耐热性能,如下述实施例进一步给予详加说明与描述。[0044] 实施例I[0045] 将固含量为60%的聚四氟乙烯分散乳液用去离子水调节粘度为20mPa-s (20°C), 然后用氨水调节PH值至11,搅拌混合均匀。[0046] 用上述调节好的聚四氟乙烯分散乳液浸溃厚度为40微米、孔隙率为92%的ePTFE 薄膜,然后送入烘箱于280°C烘烤,除去水分和助剂(乳化剂、分散剂),制作成预浸料,预浸料厚度为51微米,该制成的预浸料没有裂纹。[0047] 取5张上述的预浸料相叠合,上下各压覆一张铜箔,放进压机进行热压制得所述高频电路基板,热压温度为350°C 〜400°C,热压压力为70Kg/cm2。测试该制得的高频电路基板,介电常数为2.08 (10GHZ),介质损耗角正切为0.0002 (IOGHZ)0[0048] 实施例2[0049] 将固含量为60%的聚四氟乙烯分散乳液用去离子水调节粘度为15mPa-s (20°C), 然后用氨水调节PH值至11左右,搅拌混合均匀。将熔融型的二氧化硅粉末(硅微粉和PTFE 的重量比为I :1)加入以上乳液中,搅拌使二氧化硅均一的分散在乳液中,制得可浸溃的胶液。[0050] 用上述调节好的胶液浸溃厚度为300微米、孔隙率为95%的ePTFE薄膜,然后送入烘箱于280°C烘烤,除去水分和助剂(乳化剂、分散剂),制作成预浸料,该制成的预浸料厚度为308微米,没有裂纹。[0051] 取上述的预浸料I张,上下各压覆一张铜箔,放进压机进行热压制得所述高频电路基板,温度为380°C,压力为70Kg/cm2。测试该制得的高频电路基板,介电常数为2. 53 (10GHZ),介质损耗角正切为O. 0003 (IOGHZ)ο[0052] 实施例3[0053] 将固含量为60%的聚四氟乙烯分散乳液用去离子水调节粘度为15mPa-s (20°C), 然后用氨水调节PH值至11左右,搅拌混合均匀。将熔融型的二氧化硅粉末(硅微粉和PTFE 的重量比为I :1)加入以上乳液中,搅拌使二氧化硅均一的分散在乳液中,制得可浸溃的胶液。[0054] 用上述调节好的胶液浸溃厚度为120微米、孔隙率为95%的填充有熔融二氧化硅填料的ePTFE薄膜(薄膜中熔融二氧化硅填料的含量为50%),然后送入烘箱于280°C烘烤, 除去水分和助剂(乳化剂、分散剂),制作成预浸料,该制成的预浸料厚度为128微米,没有裂纹。[0055] 取上述的预浸料I张,上下各压覆一张铜箔,放进压机进行热压制得所述高频电路基板,温度为380°C,压力为lOOKg/cm2。测试该制得的高频电路基板,介电常数为2. 65 (10GHZ),介质损耗角正切为O. 0003 (IOGHZ)ο[0056] 比较例I[0057] 将双酚A环氧树脂(环氧树脂A)、溴化环氧树脂(环氧树脂B)溶解在二甲基甲酰胺中,并添加相对于环氧树脂O. 7摩尔比胺当量的双氰胺作固化剂和适量2-MI (2-甲基咪唑)做促进剂,然后在室温下混合得到胶液。[0058] 用以上胶液浸溃厚度为40微米、孔隙率为92%的ePTFE薄膜,然后送入烘箱于 155°C烘烤,除去溶剂二甲基甲酰胺,制作成厚度为54微米的预浸料。[0059] 取5张上述的预浸料相叠合,上下各压覆一张铜箔,放进压机进行热压制得所述高频电路基板,固化温度为177°C,固化压力为50Kg/cm2,固化时间为90分钟。测试该制得的高频电路基板,介电常数为3. 54 (10GHZ),介质损耗角正切为0.008 (IOGHZ)0[0060] 比较例2[0061] 将用二酐和二胺合成的聚酰亚胺树脂溶解在二甲基甲酰胺中,并加入适量的三苯基膦作为固化促进剂,制作成胶液。[0062] 用以上胶液浸溃厚度为40微米、孔隙率为92%的ePTFE薄膜,然后送入烘箱于 155°C烘烤,除去溶剂二甲基甲酰胺,制作成厚度为50微米的预浸料。[0063] 取5张上述的预浸料相叠合,上下各压覆一张铜箔,放进压机进行热压制得所述高频电路基板,固化温度为260°C,固化压力为50Kg/cm2,固化时间为120分钟。测试该制得的高频电路基板,介电常数为3. 32 (106瓜),介质损耗角正切为0.006 (IOGHZ)0[0064] 以上实施例和比较例皆参照IPC4101标准对覆铜板进行检测,介电性能的检测方法采用 SPDR (splite post dielectric resonator)法进行测试,测试条件为 A 态,10GHz。[0065] 从以上实施例1、2、3可以看出,所制作的预浸料厚度可以调节,且没有裂纹,制得的高频电路基板材料介电常数和介质损耗角低,高频性能好。另外,因没有采用编织纤维做增强材料,基板内部的均匀性很好,在X/Y方向介电常数不存在差异。从比较例可以看出, 因为使用了介质损耗角正切大的热固性树脂和多孔隙的ePTFE薄膜配合使用,制成的电路基板的介质损耗角正切比采用热塑性的氟聚合物树脂和多孔隙的ePTFE薄膜配合使用的电路基板的介电常数大很多。因此热塑性的氟聚合物树脂和多孔隙的ePTFE薄膜配合使用的电路基板具有更加优异的高频性能,在高频电路的信号传输中效果更好。[0066] 以上实施例,并非对本发明的组合物作任何限制,凡是依据本发明的技术实质或组合物成份或含量对以上实施例所作的任何细微修改、等同变化与修饰,均仍属于本发明技术方案的范围内。

Claims (6)

1. 一种复合材料,其特征在于,其组成物包括: (1)具有低介电损耗的氟聚合物分散乳液; (2)多孔隙的膨胀聚四氟乙烯薄膜 '及 (3)粉末填料; 所述多孔隙的膨胀聚四氟乙烯薄膜是通过膨胀拉伸方法制作而成,其孔径为I〜100 μ m,孔隙率为30〜98%,厚度为O. 5〜300 μ m ; 所述粉末填料含量占具有低介电损耗的氟聚合物分散乳液和粉末填料总量的O〜70体积% ;粉末填料的粒径中度值为O. 01-15 μ m,最大粒径不超过100 μ m ; 所述具有低介电损耗的氟聚合物为聚四氟乙烯、四氟乙烯-全氟烷氧基乙烯基醚共聚物、及全氟乙烯丙烯共聚物中的一种或多种; 所述粉末填料选自结晶型二氧化硅、熔融型的二氧化硅、球型二氧化硅、氧化铝、钛酸锶、钛酸钡、钛酸锶钡、氮化硼、氮化铝、碳化硅、二氧化钛、玻璃粉、玻璃短切纤维、滑石粉、云母粉、碳黑、碳纳米管、金属粉、及聚苯硫醚中的一种或多种。
2.如权利要求I所述的复合材料,其特征在于,所述多孔隙的膨胀聚四氟乙烯薄膜由聚四氟乙烯树脂制成,该聚四氟乙烯树脂不添加或添加有陶瓷填料。
3.如权利要求I所述的复合材料,其特征在于,还包括(4)助剂,该助剂包括有乳化剂及分散剂。
4. 一种使用如权利要求I所述的复合材料制作的高频电路基板,包括:数张相互叠合的预浸料及分别压覆于其两侧的金属箔,其特征在于,该数张预浸料均由所述复合材料制作。
5. 一种制作如权利要求4所述的高频电路基板的方法,其特征在于,包括下述步骤: 步骤I、称取复合材料的组成物; 步骤2、将具有低介电损耗的氟聚合物分散乳液,用水稀释至适当的粘度,然后用氨水调节PH值至8-12,将粉末填料和助剂混合,加入到上述调节好的分散乳液中,搅拌混合,使粉末填料均一的分散在其中,制得胶液; 步骤3、用上述胶液浸溃多孔隙的膨胀聚四氟乙烯薄膜,并控制到合适的厚度,然后于80〜30(TC烘烤去除水分及助剂,形成预浸料; 步骤4、将上述的预浸料数张相叠合,上下各压覆一张金属箔,放进压机进行热压制得所述高频电路基板,热压温度为350〜400°C,热压压力为25〜lOOKg/cm2。
6.如权利要求5所述的高频电路基板的制作方法,其特征在于,所述胶液的固体含量为30〜80% ;所述胶液在多孔隙的膨胀聚四氟乙烯薄膜表面上形成氟聚合物树脂层,其厚度控制在20微米以下。
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US10194528B2 (en) 2019-01-29
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