CN117596783A - 一种高频碳氢覆铜板及其制备方法 - Google Patents
一种高频碳氢覆铜板及其制备方法 Download PDFInfo
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- CN117596783A CN117596783A CN202311649736.7A CN202311649736A CN117596783A CN 117596783 A CN117596783 A CN 117596783A CN 202311649736 A CN202311649736 A CN 202311649736A CN 117596783 A CN117596783 A CN 117596783A
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- copper
- clad plate
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 46
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- QVCDBOQTJPSXRP-UHFFFAOYSA-N 4-[4-(aminomethyl)phenyl]phenol Chemical compound C1=CC(CN)=CC=C1C1=CC=C(O)C=C1 QVCDBOQTJPSXRP-UHFFFAOYSA-N 0.000 claims description 7
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- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 3
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
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- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
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Abstract
本发明涉及覆铜板技术领域,具体为一种高频碳氢覆铜板及其制备方法。所述高频碳氢树脂胶液包括以下重量组分:碳氢树脂80‑100份、改性双马来酰亚胺树脂30‑50份、丁酮20‑30份、甲苯80‑100份、氰酸酯20‑40份、引发剂2‑6份、阻燃剂15‑30份、抗氧化剂0.1‑5份、填料20‑40份。本发明通过将碳氢树脂和改性双马来酰亚胺树脂混合均匀,并结合阻燃剂、填料及多种助剂的共同作用,制得高频碳氢树脂胶液。使用本发明所得的高频碳氢树脂胶液制得的覆铜板不仅具有低介电常数、低介电损耗,同时赋予其优异的阻燃性能,从而延长覆铜板的使用寿命。
Description
技术领域
本发明涉及覆铜板技术领域,具体为一种高频碳氢覆铜板及其制备方法。
背景技术
随着电子通信技术的不断发展,高频电路的需求量也越来越大。碳氢树脂是一种常用的覆铜板材料,具有良好的导电性能和高频特性,因此被广泛应用于高频电路中。
传统的覆铜板通常使用环氧树脂作为基材,但其高频性能和阻燃性能有限。与传统的覆铜板相比,碳氢覆铜板具有较低的介电常数和损耗因子,可以有效减小信号传输过程中的能量损耗,提高信号传输的稳定性和可靠性。然而,由于碳氢树脂的特殊性质,制备过程相对复杂,需要控制好树脂的含量和均匀性,以保证覆铜板的性能稳定。同时,碳氢树脂的阻燃性能较差,在受到热源或火焰作用时,容易燃烧并释放有毒气体和烟雾,对人身安全和环境造成潜在风险。
因此,我们提出一种高频碳氢覆铜板及其制备方法。
发明内容
本发明的目的在于提供一种高频碳氢覆铜板及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种高频碳氢覆铜板的制备方法,包括以下步骤:
S1:将4'-氨甲基联苯基-4-酚和三乙胺混合均匀,加入丁酮混合,升温至60-70℃,滴加二对甲苯基二氯硅烷,1-2h滴完,升温至75-85℃,回流反应10-12h,经过滤、洗涤、重结晶,制得中间体;将中间体、马来酸酐和甲苯混合均匀,于室温下反应6-8h,经减压蒸馏、多次纯化,制得改性双马来酰亚胺树脂;
S2:将碳氢树脂和改性双马来酰亚胺树脂混合均匀,升温至50-70℃,加入丁酮、甲苯、氰酸酯、引发剂、阻燃剂、抗氧化剂、填料混合均匀,制得高频碳氢树脂胶液;
S3:将电子玻璃纤维布浸渍在高频碳氢树脂胶液中,进行浸胶处理,取出,于140-160℃下烘烤5-10min,制得半固化片;
S4:将4-8片半固化片重叠在一起,制得重叠片,在重叠片的上表面、下表面各放置一张铜箔,进行加热加压,冷却至室温,制得覆铜板。
进一步的,所述S1中4'-氨甲基联苯基-4-酚和三乙胺的质量比为1:(0.5-0.6)。
进一步的,所述S1中丁酮的质量为4'-氨甲基联苯基-4-酚质量的1-2倍。
进一步的,所述S1中二对甲苯基二氯硅烷的质量为4'-氨甲基联苯基-4-酚质量的0.7-0.8倍。
进一步的,所述S1中中间体、马来酸酐和甲苯的质量比为1:(0.25-0.30):(1.0-1.5)。
进一步的,所述S2中高频碳氢树脂胶液包括以下重量组分:碳氢树脂80-100份、改性双马来酰亚胺树脂30-50份、丁酮20-30份、甲苯80-100份、氰酸酯20-40份、引发剂2-6份、阻燃剂15-30份、抗氧化剂0.1-5份、填料20-40份。
进一步的,所述碳氢树脂由50-60质量份1,2-聚丁二烯、30-40质量份氢化苯乙烯-丁二烯嵌段共聚物组成。
进一步的,所述1,2-聚丁二烯的分子量为2000-7000,所述氢化苯乙烯-丁二烯嵌段共聚物的分子量为20000-250000,苯乙烯含量为10-40%,甲苯溶液粘度200-5000mpas,硬度70-88,氢化度≥97%。
进一步的,所述氰酸酯为双酚M型氰酸酯单体。
进一步的,所述引发剂由1-2质量份1,3-双丁基过氧异丙基苯、1-4质量份过氧化二叔丁基组成。
进一步的,所述阻燃剂的制备方法如下:
步骤(1):将八乙烯基倍半硅氧烷和四氢呋喃混合均匀,加入间氯过氧苯甲酸与二氯甲烷的混合溶液,搅拌均匀,升温至40-50℃,冷凝回流46-48h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和甲苯混合均匀,升温至75-85℃,加入偶氮二异丁腈混合均匀,保温反应10-12h,降温至40-50℃,滴加硼酸溶液,1-2h滴完,反应1-2h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
在上述技术方案中,通过氧化八乙烯基倍半硅氧烷,可以生成环氧基倍半硅氧烷;9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物的P-H键可以与环氧基倍半硅氧烷中的环氧基团发生反应,生成-OH基团,引入P元素;然后,将硼酸加入反应体系,与-OH基团发生反应,引入B元素,制得阻燃剂,具有优异的阻燃效果。
进一步的,所述步骤(1)中八乙烯基倍半硅氧烷和四氢呋喃的质量比为1:(10-12)。
进一步的,所述步骤(1)中间氯过氧苯甲酸与二氯甲烷的质量比为1:(3-4),间氯过氧苯甲酸的质量为八乙烯基倍半硅氧烷质量的2.5-3.0倍。
进一步的,所述步骤(2)中环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和甲苯的质量比为1:(3.0-3.2):(4-5)。
进一步的,所述步骤(2)中偶氮二异丁腈的质量为环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物总质量的0.5-1.5%。
进一步的,所述步骤(2)中硼酸溶液的浓度为4-5wt%,用量为环氧基倍半硅氧烷质量的50-60%。
进一步的,所述抗氧化剂为亚磷酸三(2,4-二叔丁基苯基)酯。
进一步的,所述填料由10-20质量份熔融硅微粉、10-20质量份二氧化锆组成。
进一步的,所述S3中浸胶处理工艺条件为:温度25-50℃,时间5-15min,高频碳氢树脂胶液与电子玻璃纤维布的质量比为1:(5-10)。
进一步的,所述S4中加热加压工艺条件为:温度190-220℃,压力2-6MPa,时间2-4h。
与现有技术相比,本发明的有益效果如下:
1、本发明的一种高频碳氢覆铜板及其制备方法,将4'-氨甲基联苯基-4-酚的羟基和二对甲苯基二氯硅烷的氯基团发生反应,引入了键能较高且柔顺性较好的硅氧烷结构,制得中间体,将马来酸酐与中间体中的-NH2键发生反应,制得改性双马来酰亚胺。通过将马来酰亚胺与有机硅烷结构相结合,不仅可以提高材料的可成型加工性和韧性,同时降低了马来酰亚胺树脂的介电常数、介电损耗和热膨胀系数,从而改善了材料的介电性能。
2、本发明的一种高频碳氢覆铜板及其制备方法,通过氧化八乙烯基倍半硅氧烷,可以生成环氧基倍半硅氧烷;9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物的P-H键可以与环氧基倍半硅氧烷中的环氧基团发生反应,生成-OH基团,引入P元素;然后,将硼酸加入反应体系,与-OH基团发生反应,引入B元素,制得含Si、P、B元素的阻燃剂,具有优异的阻燃性能。通过这些元素的协同阻燃效果,材料的阻燃性能得到显著提升,其中Si元素可以通过在燃烧时生成硅-碳阻隔层,起到阻燃效果;P元素可以通过形成磷氧酸盐等化合物,阻碍燃烧过程中的热传导和气相燃烧反应,起到阻燃的作用;B元素可以通过形成硼氧化物等化合物,吸收燃烧过程中的热量,降低燃烧温度,减缓燃烧速率,从而提高材料的阻燃性能。同时该阻燃剂具有笼状的硅氧烷高度对称结构,具有较低的介电常数和介电损耗,不仅可以提高覆铜板的阻燃性能,同时,能够赋予其优异的介电性能。
3、本发明的一种高频碳氢覆铜板及其制备方法,将碳氢树脂和改性双马来酰亚胺树脂混合均匀,并结合丁酮、甲苯、氰酸酯、引发剂、阻燃剂、抗氧化剂、填料的共同作用,制得的高频碳氢树脂胶液具有良好的粘附性、介电性能、阻燃性和抗氧化性。使用本发明的高频碳氢覆铜板制备方法,可以获得具有低介电常数、低介电损耗、良好的阻燃性和抗氧化性能的覆铜板,从而延长其使用寿命,提高电子产品的性能和可靠性。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本实施例中1,2-聚丁二烯:分子量为2000-7000上海麦克林生化科技股份有限公司;氢化苯乙烯-丁二烯嵌段共聚物:美国科腾FG1901,分子量为20000-250000,苯乙烯含量为10-40%,甲苯溶液粘度200-5000mpas,硬度70-88,氢化度≥97%,来源于上海阜润塑化科技有限公司;双酚M型氰酸酯单体:含量98.5%,来源于湖北嘉慧兴诚生物科技有限公司;熔融硅微粉:400-600目,来源于东海县晶精硅产品加工厂;二氧化锆:30-100nm,来源于江苏天行新材料有限公司提供;电子玻璃纤维布:2116型,来源于河间市中驰嘉业保温材料有限公司;铜箔:T2紫铜,厚度6μm,来源于温州宏丰电工合金股份有限公司。
以下实施例与对比例中1份等于10g。
实施例1:一种高频碳氢覆铜板的制备方法,包括以下工艺:
S1:将30份4'-氨甲基联苯基-4-酚和15份三乙胺混合均匀,加入30份丁酮混合,升温至60℃,滴加21份二对甲苯基二氯硅烷,1h滴完,升温至75℃,回流反应10h,经过滤、洗涤、重结晶,制得中间体;将30份中间体、7.5份马来酸酐和30份甲苯混合均匀,于室温下反应6h,经减压蒸馏、多次纯化,制得改性双马来酰亚胺树脂;
S2:将50份1,2-聚丁二烯、30份氢化苯乙烯-丁二烯嵌段共聚物和30份改性双马来酰亚胺树脂混合均匀,升温至50℃,加入20份丁酮、80份甲苯、20份双酚M型氰酸酯单体、1份1,3-双丁基过氧异丙基苯、1份过氧化二叔丁基、15份阻燃剂、0.1份亚磷酸三(2,4-二叔丁基苯基)酯、10份熔融硅微粉、10份二氧化锆混合均匀,制得高频碳氢树脂胶液;
S3:将电子玻璃纤维布浸渍在高频碳氢树脂胶液中,进行浸胶处理(温度25℃,时间5min,高频碳氢树脂胶液与电子玻璃纤维布的质量比为1:5),取出,于140℃下烘烤10min,制得半固化片;
S4:将4片半固化片重叠在一起,制得重叠片,在重叠片的上表面、下表面各放置一张铜箔,在温度190℃,压力2MPa,时间2h的条件下进行加热加压,冷却至室温,制得覆铜板;
所述阻燃剂的制备工艺如下:
步骤(1):将5份八乙烯基倍半硅氧烷和50份四氢呋喃混合均匀,加入7.5份间氯过氧苯甲酸与22.5份二氯甲烷的混合溶液,搅拌均匀,升温至40℃,冷凝回流46h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将5份环氧基倍半硅氧烷、15份9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和20份甲苯混合均匀,升温至75℃,加入0.1份偶氮二异丁腈混合均匀,保温反应10h,降温至40℃,滴加2.5份4wt%硼酸溶液,1h滴完,反应1h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
实施例2:一种高频碳氢覆铜板的制备方法,包括以下工艺:
S1:将40份4'-氨甲基联苯基-4-酚和22份三乙胺混合均匀,加入60份丁酮混合,升温至65℃,滴加30份二对甲苯基二氯硅烷,1.5h滴完,升温至80℃,回流反应11h,经过滤、洗涤、重结晶,制得中间体;将40份中间体、11份马来酸酐和50份甲苯混合均匀,于室温下反应7h,经减压蒸馏、多次纯化,制得改性双马来酰亚胺树脂;
S2:将55份1,2-聚丁二烯、35份氢化苯乙烯-丁二烯嵌段共聚物和40改性双马来酰亚胺树脂混合均匀,升温至60℃,加入25份丁酮、90份甲苯、30份双酚M型氰酸酯单体、1.5份1,3-双丁基过氧异丙基苯、2份过氧化二叔丁基、20份阻燃剂、3份亚磷酸三(2,4-二叔丁基苯基)酯、15份熔融硅微粉、15份二氧化锆混合均匀,制得高频碳氢树脂胶液;
S3:将电子玻璃纤维布浸渍在高频碳氢树脂胶液中,进行浸胶处理(温度40℃,时间10min,高频碳氢树脂胶液与电子玻璃纤维布的质量比为1:8),取出,于150℃下烘烤8min,制得半固化片;
S4:将6片半固化片重叠在一起,制得重叠片,在重叠片的上表面、下表面各放置一张铜箔,在温度200℃,压力4MPa,时间3h的条件下进行加热加压,冷却至室温,制得覆铜板;
所述阻燃剂的制备工艺如下:
步骤(1):将7份八乙烯基倍半硅氧烷和77份四氢呋喃混合均匀,加入20份间氯过氧苯甲酸与70份二氯甲烷的混合溶液,搅拌均匀,升温至45℃,冷凝回流47h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将6.5份环氧基倍半硅氧烷、20份9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和30份甲苯混合均匀,升温至80℃,加入0.27份偶氮二异丁腈混合均匀,保温反应11h,降温至45℃,滴加3.6份4.5wt%硼酸溶液,1.5h滴完,反应1.5h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
实施例3:一种高频碳氢覆铜板的制备方法,包括以下工艺:
S1:将50份4'-氨甲基联苯基-4-酚和30份三乙胺混合均匀,加入100份丁酮混合,升温至70℃,滴加40份二对甲苯基二氯硅烷,2h滴完,升温至85℃,回流反应12h,经过滤、洗涤、重结晶,制得中间体;将50份中间体、15份马来酸酐和75份甲苯混合均匀,于室温下反应8h,经减压蒸馏、多次纯化,制得改性双马来酰亚胺树脂;
S2:将60份1,2-聚丁二烯、40份氢化苯乙烯-丁二烯嵌段共聚物和50份改性双马来酰亚胺树脂混合均匀,升温至70℃,加入30份丁酮、100份甲苯、40份双酚M型氰酸酯单体、2份1,3-双丁基过氧异丙基苯、4份过氧化二叔丁基、30份阻燃剂、5份亚磷酸三(2,4-二叔丁基苯基)酯、20份熔融硅微粉、20份二氧化锆混合均匀,制得高频碳氢树脂胶液;
S3:将电子玻璃纤维布浸渍在高频碳氢树脂胶液中,进行浸胶处理(温度50℃,时间15min,高频碳氢树脂胶液与电子玻璃纤维布的质量比为1:10),取出,于160℃下烘烤5min,制得半固化片;
S4:将8片半固化片重叠在一起,制得重叠片,在重叠片的上表面、下表面各放置一张铜箔,在温度220℃,压力6MPa,时间4h的条件下进行加热加压,冷却至室温,制得覆铜板;
所述阻燃剂的制备工艺如下:
步骤(1):将10份八乙烯基倍半硅氧烷和120份四氢呋喃混合均匀,加入30份间氯过氧苯甲酸与120份二氯甲烷的混合溶液,搅拌均匀,升温至50℃,冷凝回流48h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将10份环氧基倍半硅氧烷、32份9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和50份甲苯混合均匀,升温至85℃,加入0.63份偶氮二异丁腈混合均匀,保温反应12h,降温至50℃,滴加6份5wt%硼酸溶液,2h滴完,反应2h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
对比例1:所述S2中高频碳氢树脂胶液包括以下重量组分:50份1,2-聚丁二烯、30份氢化苯乙烯-丁二烯嵌段共聚物、双马来酰亚胺树脂30份、丁酮20份、甲苯80份、双酚M型氰酸酯单体20份、1份1,3-双丁基过氧异丙基苯、1份过氧化二叔丁基、15份阻燃剂、0.1份亚磷酸三(2,4-二叔丁基苯基)酯、10份熔融硅微粉、10份二氧化锆;与实施例1相比,对比例1将改性双马来酰亚胺树脂替换成普通的双马来酰亚胺树脂(来源于武汉华翔科洁生物技术有限公司),其余步骤、工艺与实施例1相同。
对比例2:所述S2中高频碳氢树脂胶液包括以下重量组分:50份1,2-聚丁二烯、30份氢化苯乙烯-丁二烯嵌段共聚物、改性双马来酰亚胺树脂30份、丁酮20份、甲苯80份、双酚M型氰酸酯单体20份、1份1,3-双丁基过氧异丙基苯、1份过氧化二叔丁基、15份十溴二苯乙烷、0.1份亚磷酸三(2,4-二叔丁基苯基)酯、10份熔融硅微粉、10份二氧化锆;与实施例1相比,对比例2不包括阻燃剂的制备工艺,将S2中的阻燃剂替换成十溴二苯乙烷;其余步骤、工艺与实施例1相同。
对比例3:所述S2中高频碳氢树脂胶液包括以下重量组分:50份1,2-聚丁二烯、30份氢化苯乙烯-丁二烯嵌段共聚物、改性双马来酰亚胺树脂5份、丁酮20份、甲苯80份、双酚M型氰酸酯单体20份、1份1,3-双丁基过氧异丙基苯、1份过氧化二叔丁基、15份阻燃剂、0.1份亚磷酸三(2,4-二叔丁基苯基)酯、10份熔融硅微粉、10份二氧化锆;与实施例1相比,对比例3添加5份改性双马来酰亚胺树脂,将所述阻燃剂的制备工艺删掉,其余步骤、工艺与实施例2相同。
对比例4:一种高频碳氢覆铜板的制备方法,包括以下工艺:
所述阻燃剂的制备工艺如下:
步骤(1):将7份八乙烯基倍半硅氧烷和77份四氢呋喃混合均匀,加入20份间氯过氧苯甲酸与70份二氯甲烷的混合溶液,搅拌均匀,升温至45℃,冷凝回流47h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将6.5份环氧基倍半硅氧烷、6.5份9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和6.5份甲苯混合均匀,升温至80℃,加入0.27份偶氮二异丁腈混合均匀,保温反应11h,降温至45℃,滴加3.6份4.5wt%硼酸溶液,1.5h滴完,反应1.5h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
与实施例2相比,对比例4的步骤(2)中环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和甲苯的质量比为1:1:1,其余步骤与实施例2相同。
实验
取实施例1-3、对比例1-4中得到的覆铜板,制得试样,分别对其性能进行检测并记录检测结果:
按照IPC-TM650-2.5.5.9标准测定介电常数和介电损耗因子,实验步骤:将覆铜板试样切割成50mm×50mm大小的尺寸,使用SPDR(分离式介电谐振器)进行测量,测试频率为10GHz,启动测试仪器,记录数据。
按照美国UL-94标准的垂直燃烧法测定阻燃性,实验步骤:将覆铜板试样切割成100mm×10mm大小的尺寸,将其垂直放置在燃烧装置的夹具上,确保试样的下端离开火焰源约20mm,使用火焰源点燃试样的下端,观察试样的燃烧特性,包括燃烧时间、滴落情况、火焰蔓延情况等,根据试样的燃烧特性,分为以下几种等级:V-0等级:试样的燃烧时间不超过10秒钟,火焰熄灭后不产生火花或燃烧滴落,并且试样上部的燃烧扩散距离不超过50mm;V-1等级:试样的燃烧时间不超过30秒钟,火焰熄灭后不产生火花或燃烧滴落,并且试样上部的燃烧扩散距离不超过75mm;V-2等级:试样的燃烧时间不超过30秒钟,火焰熄灭后不产生火花或燃烧滴落,并且试样上部的燃烧扩散距离不超过125mm。
测试结果
根据上表中的数据,可以清楚得到以下结论:
1、与对比例1相比,实施例1-3所得产物的介电常数、介电损耗均降低,说明相较于普通的双马来酰亚胺树脂,本发明制备的改性双马来酰亚胺树脂能够显著提高覆铜板的介电性能。
2、与实施例1-3相比,对比例2所得产物的阻燃性降低,可知相较于十溴二苯乙烷,本发明制备的阻燃剂的阻燃效果更好。
3、与实施例1-3相比,对比例3所得产物的介电性能下降,可知添加本发明中所述范围内的改性双马来酰亚胺树脂配比,可以改善覆铜板的介电性能;对比例4所述产物的阻燃性能下降,说明本发明的阻燃剂受其制备工艺中各试剂配比的影响,选择在所述范围内的试剂配比,可以提高阻燃剂的阻燃性能,从而延长覆铜板的使用寿命。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程方法物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程方法物品或者设备所固有的要素。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高频碳氢覆铜板的制备方法,其特征在于:包括以下步骤:
S1:将4'-氨甲基联苯基-4-酚和三乙胺混合均匀,加入丁酮混合,升温至60-70℃,滴加二对甲苯基二氯硅烷,1-2h滴完,升温至75-85℃,回流反应10-12h,经过滤、洗涤、重结晶,制得中间体;将中间体、马来酸酐和甲苯混合均匀,于室温下反应6-8h,经减压蒸馏、多次纯化,制得改性双马来酰亚胺树脂;
S2:将碳氢树脂和改性双马来酰亚胺树脂混合均匀,升温至50-70℃,加入丁酮、甲苯、氰酸酯、引发剂、阻燃剂、抗氧化剂、填料混合均匀,制得高频碳氢树脂胶液;
S3:将电子玻璃纤维布浸渍在高频碳氢树脂胶液中,进行浸胶处理,取出,于140-160℃下烘烤5-10min,制得半固化片;
S4:将4-8片半固化片重叠在一起,制得重叠片,在重叠片的上表面、下表面各放置一张铜箔,进行加热加压,冷却至室温,制得覆铜板。
2.根据权利要求1所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述S1中二对甲苯基二氯硅烷的质量为4'-氨甲基联苯基-4-酚质量的0.7-0.8倍。
3.根据权利要求1所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述S2中高频碳氢树脂胶液包括以下重量组分:碳氢树脂80-100份、改性双马来酰亚胺树脂30-50份、丁酮20-30份、甲苯80-100份、氰酸酯20-40份、引发剂2-6份、阻燃剂15-30份、抗氧化剂0.1-5份、填料20-40份。
4.根据权利要求3所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述碳氢树脂由50-60质量份1,2-聚丁二烯、30-40质量份氢化苯乙烯-丁二烯嵌段共聚物组成。
5.根据权利要求3所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述引发剂由1-2质量份1,3-双丁基过氧异丙基苯、1-4质量份过氧化二叔丁基组成。
6.根据权利要求3所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述阻燃剂的制备工艺如下:
步骤(1):将八乙烯基倍半硅氧烷和四氢呋喃混合均匀,加入间氯过氧苯甲酸与二氯甲烷的混合溶液,搅拌均匀,升温至40-50℃,冷凝回流46-48h,进行冰浴降温,经过滤、多次洗涤,旋蒸蒸发后,制得环氧基倍半硅氧烷;
步骤(2):在氮气保护下,将环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和甲苯混合均匀,升温至75-85℃,加入偶氮二异丁腈混合均匀,保温反应10-12h,降温至40-50℃,滴加硼酸溶液,1-2h滴完,反应1-2h,冷却至室温,经过滤、洗涤、干燥后,制得阻燃剂。
7.根据权利要求6所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述步骤(1)中间氯过氧苯甲酸与二氯甲烷的质量比为1:(3-4),间氯过氧苯甲酸的质量为八乙烯基倍半硅氧烷质量的2.5-3.0倍。
8.根据权利要求6所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述步骤(2)中环氧基倍半硅氧烷、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和甲苯的质量比为1:(3.0-3.2):(4-5)。
9.根据权利要求1所述的一种高频碳氢覆铜板的制备方法,其特征在于:所述S4中加热加压工艺条件为:温度190-220℃,压力2-6MPa,时间2-4h。
10.根据权利要求1-9任一项所述制备方法制得的一种高频碳氢覆铜板。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11349789A (ja) * | 1998-06-08 | 1999-12-21 | Toppan Printing Co Ltd | 多層プリント配線板用難燃性絶縁樹脂組成物 |
JP2001311081A (ja) * | 2000-04-27 | 2001-11-09 | Kanegafuchi Chem Ind Co Ltd | 難燃剤 |
CN105315492A (zh) * | 2015-12-04 | 2016-02-10 | 南昌航空大学 | 一种基于笼型倍半硅氧烷的磷硅硼阻燃剂及其制备方法 |
CN110218436A (zh) * | 2019-06-19 | 2019-09-10 | 南亚新材料科技股份有限公司 | 一种低介电树脂组合物及其制备方法 |
CN110317541A (zh) * | 2019-06-19 | 2019-10-11 | 南亚新材料科技股份有限公司 | 一种粘结片以及高速覆铜板的制备方法 |
CN116925446A (zh) * | 2023-07-17 | 2023-10-24 | 江苏耀鸿电子有限公司 | 一种覆铜板用高导热碳氢树脂及其制备方法 |
-
2023
- 2023-12-05 CN CN202311649736.7A patent/CN117596783A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11349789A (ja) * | 1998-06-08 | 1999-12-21 | Toppan Printing Co Ltd | 多層プリント配線板用難燃性絶縁樹脂組成物 |
JP2001311081A (ja) * | 2000-04-27 | 2001-11-09 | Kanegafuchi Chem Ind Co Ltd | 難燃剤 |
CN105315492A (zh) * | 2015-12-04 | 2016-02-10 | 南昌航空大学 | 一种基于笼型倍半硅氧烷的磷硅硼阻燃剂及其制备方法 |
CN110218436A (zh) * | 2019-06-19 | 2019-09-10 | 南亚新材料科技股份有限公司 | 一种低介电树脂组合物及其制备方法 |
CN110317541A (zh) * | 2019-06-19 | 2019-10-11 | 南亚新材料科技股份有限公司 | 一种粘结片以及高速覆铜板的制备方法 |
CN116925446A (zh) * | 2023-07-17 | 2023-10-24 | 江苏耀鸿电子有限公司 | 一种覆铜板用高导热碳氢树脂及其制备方法 |
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