CN112719264A - 一种聚苯乙烯/银复合微球的制备方法 - Google Patents
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Abstract
本发明公开了一种聚苯乙烯/银复合微球的制备方法,属于材料制备技术领域。本发明所述方法先对PS(聚苯乙烯)微球表面进行粗化处理,然后将粗化后的PS微球进行多次敏化和镀银处理,在超声的条件下将处理后的PS微球加入到银氨溶液中,加入定量的还原剂完成PS微球表面的化学镀银;过滤、洗涤、离心,干燥后得到PS/Ag复合粒子。本发明所述的PS镀银方法,制备较为工艺、原料组成简单,易于大规模生产,制备的复合微球表面银覆盖率高,分散性较好。
Description
技术领域
本发明涉及一种聚苯乙烯/银复合微球的制备方法,属于化学镀银技术领域。
背景技术
传统的各向异性导电薄膜是用金属颗粒或有机-无机复合颗粒作为粘合聚合物基质中的填料并将其形成固体薄膜而制成的。直径为几微米的有机-无机复合粒子通常由高导电性金属(如金或银)包覆。同时,与粘着聚合物基体相比,弹性芯具有相似的热膨胀系数,并且在热压后的两个电极互连之间提供了较大的接触面积。在聚合物核中,聚苯乙烯(PS)微球具有尺寸可控、形状可控、单分散性好、官能团多样、易于高温煅烧或溶剂溶解等优点。
PS微球在做为复合材料核心时,能通过控制微球的尺寸,从而制备各种粒径和形状的复合微球,但在进行传统化学镀过程中,由于PS微球的自身性质,使得在微球表面上包覆较为困难,造成覆盖率低,分散性差。
发明内容
本发明的目的在于提供一种聚苯乙烯/银复合微球的制备方法,具体包括以下步骤:
(1)将PS微球加入三氧化铬和浓硫酸混合的粗化液中,进行粗化处理;
(2)将步骤(1)所得到的PS微球依次加入到敏化液和银氨溶液中进行敏化和镀银,所述敏化液为二水合氯化亚锡和浓盐酸的混合溶液;
(3)将步骤(2)所得到的PS微球,在步骤(2)的条件重复处理4~6次;
(4)将步骤(3)所得到的PS微球加入到银氨溶液中,在超声分散条件下,滴加还原剂水合肼,经过滤、洗涤,干燥,得PS/Ag复合填料。
优选的,本发明步骤(1)所述粗化液中三氧化铬的质量分数为2~8%,浓硫酸的质量分数为30~50%,所述浓硫酸为质量百分比浓度为98%的浓硫酸,粗化液的加入比例为50~80ml每克PS微球。
优选的,本发明步骤(1)中粗化过程的反应条件为在恒温20℃下,磁力搅拌速度为100r/min。
优选的,本发明步骤(2)所述敏化液中SnCl2·2H2O的质量分数为2~10%,浓盐酸的质量分数为2~6%,敏化液的使用量为50~80mL每克PS微球。
优选的,本发明步骤(2)中敏化过程的条件为:在恒温20℃下,磁力搅拌400r/min。
优选的,本发明步骤(2)银氨溶液中硝酸银与氨水的质量体积比为1:2~6,银氨溶液的添加量为20~40ml每克PS微球,其中PS微球与硝酸银的质量比为1:1~2。
优选的,本发明步骤(2)中镀银时的反应条件为在恒温20℃下,磁力搅拌速度为200r/min。
优选的,本发明步骤(4)中银氨溶液中硝酸银与氨水的质量体积比为1:4~10,银氨溶液的添加量为40~60ml每克PS微球,其中PS微球与硝酸银的质量比为1:1~4;每克硝酸银所需质量百分比浓度为50%的水合肼为2~4ml。
优选的,本发明步骤(4)镀银时的反应条件为在40Hz超声下,匀速滴加水合肼4min/mL;复合微球的干燥条件为恒温60℃。
本发明的有益效果:
(1)本发明工艺安全、简单有效,所制备的复合粒子具有高包覆率,良好的分散性;本发明以聚苯乙烯(PS)微球为核,制备的复合粒子,拥有者广泛的应用;例如,可以作为各项异性导电胶的导电粒子;可作为银催化反应的载体,通过调节比表面积,提高催化能力。
(2)本发明利用酸性水溶液的强氧化作用粗化PS微球表面,使PS微球的比表面积增大,以利于敏化过程中Sn2+离子的附着,提高敏化效率;另外,在粗化过程中,本发明所配置的复合氧化液会在PS微球的表面植入磺酸基团(SO3 2-);该基团带负电且是亲水基团,因此,可以提高PS微球表面的附着能力;敏化后,加入银氨,Ag+被Sn2+还原到PS微球表面;镀银过程中,Ag+将以金属Ag为原位还原中心进行还原,还原出的Ag单质附着在PS微球的表面逐渐形成一层致密的银层。PS微球化学镀银的原理示意图如图(1)所示
(3)与现有技术相比,本发明所述的PS微球化学镀银方法所获得的PS/Ag复合粒子具有高包覆率和良好的分散性;由于在粗化过程中是磺酸基团均匀分布,通过多次敏化、镀银过程也能在PS微球上还原出均匀的银生长点,作为后续微球表面原位还原的生长核心;超声辅助的化学镀,由于超声的空化作用,使得镀层覆盖率提高,复合微球的分散性也有改善。
附图说明
图1为本发明在三种实施例下的PS/Ag复合粒子的扫描电镜图;
图2为本发明的PS/Ag复合粒子的原理示意图;
图3为本发明所制备的PS/Ag复合粒子的扫描电镜图。
具体实施方式
下面结合具体实施例本发明作进一步的详细说明,但本发明的保护范围并不限于所述内容。
实施例1
一种聚苯乙烯/银复合微球的制备方法,具体包括以下步骤:
(1)将PS微球加入三氧化铬和浓硫酸混合的粗化液中,在恒温20℃,磁力搅拌速度为100r/min的条件下粗化处理4h;所述粗化液中三氧化铬的质量分数为2%,浓硫酸的质量分数为40%,所述浓硫酸为质量百分比浓度为98%的浓硫酸,粗化液的加入比例为50ml每克PS微球。
(2)将步骤(1)所得到的PS微球加入到敏化液中,在恒温20℃,磁力搅拌400r/min的条件下敏化处理20min,所述敏化液为二水合氯化亚锡和浓盐酸的混合溶液,敏化液中SnCl2·2H2O的质量分数为2%,浓盐酸的质量分数为4%,敏化液的使用量为50mL每克PS微球;然后加入到银氨溶液中,在恒温20℃,磁力搅拌速度为200r/min的条件下进行镀银,所述银氨溶液中硝酸银与氨水的质量体积比为1:4,银氨溶液的添加量为20ml每克PS微球,其中PS微球与硝酸银的质量比为1:1,重复处理4次。
(3)将步骤(2)所得到的PS微球加入到银氨溶液中,在40Hz超声下超声分散条件下,按4min/mL的滴加速度滴加还原剂水合肼,经过滤、洗涤,恒温60℃干燥,得PS/Ag复合填料;所述银氨溶液中硝酸银与氨水的质量体积比为1:8,银氨溶液的添加量为40ml每克PS微球,其中PS微球与硝酸银的质量比为1:1;每克硝酸银所需质量百分比浓度为50%的水合肼为2ml。
实施例2
一种聚苯乙烯/银复合微球的制备方法,具体包括以下步骤:
(1)将PS微球加入三氧化铬和浓硫酸混合的粗化液中,在恒温20℃,磁力搅拌速度为100r/min的条件下粗化处理4h;所述粗化液中三氧化铬的质量分数为8%,浓硫酸的质量分数为50%,所述浓硫酸为质量百分比浓度为98%的浓硫酸,粗化液的加入比例为80ml每克PS微球。
(2)将步骤(1)所得到的PS微球加入到敏化液中,在恒温20℃,磁力搅拌400r/min的条件下敏化处理20min,所述敏化液为二水合氯化亚锡和浓盐酸的混合溶液,敏化液中SnCl2·2H2O的质量分数为10%,浓盐酸的质量分数为6%,敏化液的使用量为80mL每克PS微球;然后加入到银氨溶液中,在恒温20℃,磁力搅拌速度为200r/min的条件下进行镀银,所述银氨溶液中硝酸银与氨水的质量体积比为1:6,银氨溶液的添加量为40ml每克PS微球,其中PS微球与硝酸银的质量比为1:2,重复处理5次。
(3)将步骤(2)所得到的PS微球加入到银氨溶液中,在40Hz超声下超声分散条件下,按4min/mL的滴加速度滴加还原剂水合肼,经过滤、洗涤,恒温60℃干燥,得PS/Ag复合填料;所述银氨溶液中硝酸银与氨水的质量体积比为1:10,银氨溶液的添加量为60ml每克PS微球,其中PS微球与硝酸银的质量比为1:4;每克硝酸银所需质量百分比浓度为50%的水合肼为4ml。
实施例3
一种聚苯乙烯/银复合微球的制备方法,具体包括以下步骤:
(1)将PS微球加入三氧化铬和浓硫酸混合的粗化液中,在恒温20℃,磁力搅拌速度为100r/min的条件下粗化处理4h;所述粗化液中三氧化铬的质量分数为6%,浓硫酸的质量分数为30%,所述浓硫酸为质量百分比浓度为98%的浓硫酸,粗化液的加入比例为60ml每克PS微球。
(2)将步骤(1)所得到的PS微球加入到敏化液中,在恒温20℃,磁力搅拌400r/min的条件下敏化处理20min,所述敏化液为二水合氯化亚锡和浓盐酸的混合溶液,敏化液中SnCl2·2H2O的质量分数为6%,浓盐酸的质量分数为2%,敏化液的使用量为60mL每克PS微球;然后加入到银氨溶液中,在恒温20℃,磁力搅拌速度为200r/min的条件下进行镀银,所述银氨溶液中硝酸银与氨水的质量体积比为1:2,银氨溶液的添加量为30ml每克PS微球,其中PS微球与硝酸银的质量比为1:1,重复处理6次。
(3)将步骤(2)所得到的PS微球加入到银氨溶液中,在40Hz超声下超声分散条件下,按4min/mL的滴加速度滴加还原剂水合肼,经过滤、洗涤,恒温60℃干燥,得PS/Ag复合填料;所述银氨溶液中硝酸银与氨水的质量体积比为1:4,银氨溶液的添加量为50ml每克PS微球,其中PS微球与硝酸银的质量比为1:1;每克硝酸银所需质量百分比浓度为50%的水合肼为3ml。
图1为实施例1~3的SEM图,实施例1显示图中在低浓度粗化液,较少敏化、镀银次数,和PS微球与硝酸银低质量比条件下,PS微球表面包覆率低;实施例2显示图中较高浓度粗化液,和增加一次敏化、镀银次数,和PS微球与硝酸银合适质量比条件下,PS微球表面包覆率高,微球分散性良好。实施例3显示图中低浓度的粗化液,对微球表面改性效果下降,即使提高敏化、镀银次数,和提高PS微球与硝酸银质量比条件下,微球表面银的包覆率不高,且由于硝酸银过量导致微球团聚。
如图3所示,是在上述条件下,通过超声辅助制备的Ag/PS复合微球,从SEM图中可以看出,PS微球上覆盖着均匀的银壳,包覆效果好;从微球的整体分布来看,微球的分散性也表现良好,即证明可以通过以上所述的方法制备分散性良好、包覆完整的聚苯乙烯/银复合微球。
Claims (9)
1.一种聚苯乙烯/银复合微球的制备方法,其特征在于,具体包括以下步骤:
(1)将PS微球加入三氧化铬和浓硫酸混合的粗化液中,进行粗化处理;
(2)将步骤(1)所得到的PS微球依次加入到敏化液和银氨溶液中进行敏化和镀银,所述敏化液为二水合氯化亚锡和浓盐酸的混合溶液;
(3)将步骤(2)所得到的PS微球,在步骤(2)的条件重复处理4~6次;
(4)将步骤(3)所得到的PS微球加入到银氨溶液中,在超声分散条件下,滴加还原剂水合肼,经过滤、洗涤,干燥,得PS/Ag复合填料。
2.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(1)所述粗化液中三氧化铬的质量分数为2~8%,浓硫酸的质量分数为30~50%,所述浓硫酸为质量百分比浓度为98%的浓硫酸,粗化液的加入比例为50~80ml每克PS微球。
3.根据权利要求2所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(1)中粗化过程的反应条件为在恒温20℃下,磁力搅拌速度为100r/min。
4.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(2)所述敏化液中SnCl2·2H2O的质量分数为2~10%,浓盐酸的质量分数为2~6%,敏化液的使用量为50~80mL每克PS微球。
5.根据权利要求4所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(2)中敏化过程的条件为:在恒温20℃下,磁力搅拌400r/min。
6.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(2)银氨溶液中硝酸银与氨水的质量体积比为1:2~6,银氨溶液的添加量为20~40ml每克PS微球,其中PS微球与硝酸银的质量比为1:1~2。
7.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(2)中镀银时的反应条件为在恒温20℃下,磁力搅拌速度为200r/min。
8.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(4)中银氨溶液中硝酸银与氨水的质量体积比为1:4~10,银氨溶液的添加量为40~60ml每克PS微球,其中PS微球与硝酸银的质量比为1:1~4;每克硝酸银所需质量百分比浓度为50%的水合肼为2~4ml。
9.根据权利要求1所述聚苯乙烯/银复合微球的制备方法,其特征在于:步骤(4)镀银时的反应条件为在40Hz超声下,匀速滴加水合肼4min/mL;复合微球的干燥条件为恒温60℃。
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