CN106711117B - 一种石墨烯键合银丝及其制备方法 - Google Patents

一种石墨烯键合银丝及其制备方法 Download PDF

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CN106711117B
CN106711117B CN201710054902.7A CN201710054902A CN106711117B CN 106711117 B CN106711117 B CN 106711117B CN 201710054902 A CN201710054902 A CN 201710054902A CN 106711117 B CN106711117 B CN 106711117B
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李天祥
孔杰
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Make Innovations Electronic Science And Technology Co Ltd In University Of Science And Technology Shandong
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Abstract

本发明提供了一种石墨烯键合银丝及其制备方法，种石墨烯键合银丝，由以下组分组成：石墨烯0.5%‑5%，Ag 95%‑99.5%，制备方法，包括以下步骤：S1、通过化学合成法制得银/氧化石墨烯复合粉；S2、将银/氧化石墨烯复合粉进行还原处理；S3、采用粉末冶金技术，将所述银/石墨烯复合粉进行成型、烧结处理，制得银/石墨烯复合材料；S4、真空熔炼；S5、竖式熔炼；S6、拉丝；S7、退火；S8、绕线，在银合金中添加石墨烯，显著增加了银合金的导电性，可以取代金线用于大功率的LED，环保、低成本、可控性好的生产工艺手段实现高性能石墨烯银合金丝的制备，不仅具有重要的科研价值，而且具有广泛的应用前景。

Description

一种石墨烯键合银丝及其制备方法
技术领域
本发明涉及封装用键合丝技术领域，尤其涉及一种石墨烯键合银丝及其制备方法。
背景技术
银合金作为键合丝材料具有高的反光率，低价值等优势，是LED中替代金线的理想材料。但是银合金线具有电阻率高，容易发热的缺点，因此一些大功率的LED没有办法取代金线。本发明一种石墨烯键合银丝，在银合金中添加石墨烯，显著增加了银合金的导电性，可以取代金线用于大功率的LED。
发明内容
本发明提供了一种石墨烯键合银丝及其制备方法，利用粉末冶金工艺制备石墨烯和银的合金，在高真空熔炼炉中熔化银，按比例添加石墨烯银合金，利用电磁搅拌，使石墨烯均匀分布于银溶液中，拉铸成棒，经过拉丝，退火，绕线制备出石墨烯键合银丝。
为解决上述技术问题，本发明提供了一种石墨烯键合银丝，由以下组分组成：石墨烯0.5%-5 %，Ag 95%-99.5 % 。
本发所述的一种石墨烯键合银丝的制备方法，包括以下步骤：
S1、通过化学合成法制得银/氧化石墨烯复合粉，具体为：将氧化石墨烯溶液与还原剂溶液混合，然后将该混合液与硝酸银溶液混合，获得银/氧化石墨烯复合粉的悬浊液，经沉降、洗涤、干燥获得纯净的银/氧化石墨烯复合粉；
S2、将银/氧化石墨烯复合粉进行还原处理；
S3、采用粉末冶金技术，将所述银/石墨烯复合粉进行成型、烧结处理，制得银/石墨烯复合材料；
S4、真空熔炼：将步骤3得到的银/石墨烯复合材料与的高纯银颗粒放入坩埚中，加热熔化，利用电磁搅拌，使石墨烯均匀的分布在石墨烯中，精炼一段时间后倒入石墨锭模中，冷却铸板，石墨烯在合金中的含量为0.5wt%-5wt %，加热温度为1200℃-1600℃，精炼时间为20min-30min。
S5、竖式熔炼：将步骤4得到的合金在惰性气体氩气的保护下进行熔炼，拉铸成棒材，熔炼温度为1200℃-1400℃；
S6、拉丝：拉铸后的棒材在拉丝机上逐步拉细，直至要求的直径，其拉丝过程中的模具延伸率为5%-8%，拉丝速度为0.5-15m/s；
S7、退火：退火温度为400-600℃，速度0.5-2m/s；
S8、绕线：将丝线分绕成不同长度的小轴。
作为本发明的一个优选的技术方案，所述的步骤S1的所述还原剂为抗坏血酸、葡萄糖、柠檬酸、草酸无毒环保型的一种或几种，还原剂溶液及硝酸银溶液的浓度均为0.1mol/L，氧化石墨烯溶液的质量浓度为0.5%-2%，氧化石墨烯的添加量占银/氧化石墨烯复合粉10wt%-30 wt %。
作为本发明的一个优选的技术方案，所述的S2的还原过程在氢气气氛下加热还原，加热温度300℃-700℃，加热时间3-12小时，得到银/石墨烯复合粉。
作为本发明的一个优选的技术方案，所述的粉末冶金技术包括冷等静压与烧结过程，等静压压力为0.6GPa-6GPa，烧结温度为500℃-900℃，烧结时间为3-12小时，烧结气氛为氮气。
本申请实施例中提供的一个或多个技术方案，至少具有如下技术效果或优点：
1、本发明在银合金中添加石墨烯，显著增加了银合金的导电性，可以取代金线用于大功率的LED。
2、本发明以一种环保、低成本、可控性好的生产工艺手段实现高性能石墨烯银合金丝的制备，不仅具有重要的科研价值，而且具有广泛的应用前景。
具体实施方式
为了更好的理解上述技术方案，下面将以具体的实施方式对上述技术方案进行详细的说明。
本实施例所述的原料配比：石墨烯0.5%，Ag99.5%
制备方法：
1、通过化学合成法制得银/氧化石墨烯复合粉，
基本步骤：
（1）配置0.1mol/L硝酸银溶液与0.1mol/L抗坏血酸溶液（或葡萄糖或柠檬酸或草酸的一种或几种）；
（2）取2.5L抗坏血酸溶液与250g高质量浓度为0.5%的氧化石墨烯溶液混合，离子搅拌5-10分钟，取2L硝酸银溶液加入到上述混合液中，继续离子搅拌。硝酸银与抗坏血酸发生还原反应，生成银颗粒。氧化石墨烯被银粉吸附，得到银/氧化石墨烯悬浊液。将银/氧化石墨烯悬浊液离心洗涤5-10次，冷冻干燥，得到银/氧化石墨烯混合粉。
2、 将银/氧化石墨烯复合粉在氢气气氛下加热还原，550℃加热还原3小时，得到银/石墨烯复合粉。
3、利用冷等静压技术将银/石墨烯复合粉压制成型，得到相应坯锭，将该坯锭放置于烧结炉，氮气气氛下850℃烧结10小时，得到高致密度的银/石墨烯复合材料。
4、真空熔炼，制备石墨烯银合金。
（1）按重量百分比称取银/石墨烯复合材料与高纯银颗粒，银/石墨烯复合材料5%，高纯银颗粒95%，高纯银颗粒纯度为99.999%。
（2）投料，将银/石墨烯复合材料与高纯银颗粒放入坩埚中。
（3）真空熔炼，利用电磁搅拌，使石墨烯均匀的分布在合金中。
浇铸，将合金液倒入石墨锭模中，冷却铸板。
5、竖式熔炼：将步骤4得到合金放入竖式连续熔铸机坩埚中，设定加热温度1200℃-1400℃，在惰性气体氩气的保护下进行熔炼，拉铸成棒材。
6、拉丝：拉铸后的棒材在拉丝机上逐步拉细，直至要求的直径。其拉丝过程中的模具延伸率为5%-8%，拉丝速度为0.5-15m/s。
7、退火：根据性能要求设定合适的温度进行退火。
8、绕线：将丝线分绕成长度为500米和1000米两种规格的小轴。
石墨烯键合银丝测试数据（以20um为例）
拉断力（cN） 7.00 7.20 6.80 7.40 7.20 6.90 7.58 7.60
延伸率（%） 8.52 7.90 7.84 8.00 7.81 7.71 8.79 8.62
以上所述，仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制，虽然本发明已以较佳实施例揭露如上，然而并非用以限定本发明，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。

Claims (3)

1.一种石墨烯键合银丝的制备方法，其特征在于，包括以下步骤：
S1、通过化学合成法制得银/氧化石墨烯复合粉，具体为：将氧化石墨烯溶液与还原剂溶液混合，然后将该混合液与硝酸银溶液混合，获得银/氧化石墨烯复合粉的悬浊液，经沉降、洗涤、干燥获得纯净的银/氧化石墨烯复合粉, 所述还原剂为抗坏血酸、葡萄糖、柠檬酸、草酸无毒环保型的一种或几种，还原剂溶液及硝酸银溶液的浓度均为0.1mol/L，氧化石墨烯溶液的质量浓度为0.5%-2%，氧化石墨烯的添加量占银/氧化石墨烯复合粉10wt%-30wt %；
S2、将银/氧化石墨烯复合粉进行还原处理；
S3、采用粉末冶金技术，将所述银/石墨烯复合粉进行成型、烧结处理，制得银/石墨烯复合材料；
S4、真空熔炼：将步骤3得到的银/石墨烯复合材料与的高纯银颗粒放入坩埚中，加热熔化，利用电磁搅拌，使石墨烯均匀的分布在石墨烯中，精炼一段时间后倒入石墨锭模中，冷却铸板，石墨烯在合金中的含量为0.5wt%-5wt %，加热温度为1200℃-1600℃，精炼时间为20min-30min；
S5、竖式熔炼：将步骤4得到的合金在惰性气体氩气的保护下进行熔炼，拉铸成棒材，熔炼温度为1200℃-1400℃；
S6、拉丝：拉铸后的棒材在拉丝机上逐步拉细，直至要求的直径，其拉丝过程中的模具延伸率为5%-8%，拉丝速度为0.5-15m/s；
S7、退火：退火温度为400-600℃，速度0.5-2m/s；
S8、绕线：将丝线分绕成不同长度的小轴。
2.根据权利要求1 所述的一种石墨烯键合银丝的制备方法，其特征在于，所述的S2的还原过程在氢气气氛下加热还原，加热温度300℃-700℃，加热时间3-12小时，得到银/石墨烯复合粉。
3.根据权利要求1 所述的一种石墨烯键合银丝的制备方法，其特征在于，所述的粉末冶金技术包括冷等静压与烧结过程，等静压压力为0.6GPa-6GPa，烧结温度为500℃-900℃，烧结时间为3-12小时，烧结气氛为氮气。
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