CN114724743A - 一种含纳米晶/非晶复合铜锆银粉的复合导电银浆 - Google Patents
一种含纳米晶/非晶复合铜锆银粉的复合导电银浆 Download PDFInfo
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Abstract
本发明公开一种含纳米晶/非晶复合铜锆银粉的复合导电银浆的制备方法,该方法通过纳米晶/非晶复合CuZrAg粉是用物理方法制备得到,即使用激光加热金属靶材使金属元素汽化,相比于通过改性银粉从而提高其导电性的方法。通过物理添加方法的制备工艺简单,省略了繁琐的化学反应流程,更避开了很多化学法制备纳米金属颗粒时用到的危险化学品,故本发明的安全系数远远高于大部分化学改性方法;此外,本发明的操作流程简单,纳米晶/非晶复合CuZrAg粉生产效率高,只需简单添加即可。
Description
技术领域
本发明属导电银浆领域,尤其涉及一种含纳米晶/非晶复合铜锆银粉的复合导电银浆。
背景技术
一般来说,烧结型导电银浆需要在高于500℃的温度下烧结成膜,玻璃粉或氧化物为粘结相。银粉按照粒径进行分类,平均粒径(Dav)为1-100nm为纳米银粉;0.1μm<平均粒径(Dav)<10μm为银微粉;平均粒径(Dav)>10μm为粗银粉。目前制备粉末的方法有很多,就银粉而言,可以使用物理法(液体雾化法、蒸发冷凝法),化学法(硝酸银分解热分解法、液相还原法)。其中蒸发冷凝法是制备纳米粒子的一种重要方法,所得产品粒径一般分布5-100nm之间,且得到的纳米粒子有纯度高、粒径分布窄、表面干净等优点。目前,导电银浆已广泛应用于各类电子产品,但随着电子产品向更轻、更薄、功能更强大的方向发展,对导电银浆的性能也提出了更高的要求。目前商用导电银浆的方阻为8-15mΩ/□,若能进一步提高其导电性能,则很有可能成为电子产品新一代的“宠儿”。因此,有许多研究人员在现有导电银浆的基础上进行改性,如添加微量的石墨烯,以提高银浆的导电性能。但大部分添加物的成本往往远超于导电银浆的成本,因此不具有市场竞争力,也难以推广。
发明内容
本发明的目的是提供一种含有纳米晶/非晶复合CuZrAg粉的复合导电银浆。
为了实现上述目的,本发明采用如下技术方案:
一种含纳米晶/非晶复合CuZrAg粉的复合导电银浆,由以下重量份的原料制得:
微米银粉53-58份、纳米晶/非晶复合CuZrAg粉0.5-5份,分散剂BYK0.5份、玻璃粉1份、载体40.5份,载体的配比为:松油醇40份、丁基卡必醇35.4份、丁基卡必醇醋酸酯8份、醇酯十二8份、乙基纤维素6.6份、司班85 2份。
结合图1,本发明提供了一种容器装置:包含一高真空制粉腔室,包含一个外置激光发射器,用于激发金属靶材中的原子。包含一个液氮冷却罐,用于对腔体中金属纳米颗粒的吸附沉积;包含一个方柱形收粉罐置于液氮冷却罐的下方,用于收集冷却罐上刮落的金属纳米颗粒;包含一组机械泵和分子泵,用于保证腔室内的超高真空度。
含纳米晶/非晶复合CuZrAg粉制备方法为:
将CuZrAg靶材进行表面预处理,打磨,抛光去除表面氧化层,用酒精超声清洗后,固定在高真空制粉腔体内相应位置。
将腔室密封,通过机械泵和分子泵将制粉腔内气压抽至超高真空状态(低于10-6Pa),待真空稳定后,向制粉腔内缓慢输入800Pa的高纯氦气。
向液氮冷却罐中输入液氮,直至液氮罐充满液氮。
将外置激光器瞄准腔体内的金属靶材,调整激光角度使发射出的激光垂直于靶材,同时调整激光器距离靶材的距离,使得激光发射镜头到靶材的距离在70-80cm之间。以保证激光打到靶材上的功率是最大功率。金属靶表面蒸发出的金属蒸汽或金属原子和腔室中的惰性气体氦气发生碰撞并快速降温,形成新的固相纳米粉末,由于液氮罐内超低温液氮的原因,吸附并沉积在液氮罐外侧铜辊表面。
转动铜辊旁的刮刀,将铜辊上的纳米晶/非晶复合CuZrAg粉刮落至下方的方柱形收粉罐中。
按微米银粉53-58份、纳米晶/非晶复合CuZrAg粉0.5-5份,分散剂BYK0.5、玻璃粉1、载体40.5,载体的配比为:松油醇40、丁基卡必醇35.4、丁基卡必醇醋酸酯8、醇酯十二8、乙基纤维素6.6、司班85 2的配方混合,搅拌24小时;得到含有纳米晶/非晶复合CuZrAg粉的复合导电银浆。
该方法流程简单,需要的化学药品少,可以快速高效的得到复合导电银浆,且本发明不限于添加纳米晶/非晶复合CuZrAg粉末,还可以添加其他体系/成分的纳米晶/非晶复合粉末。
本发明与现有的导电银浆的方法相比,具有如下的优点和效果:
(1)本发明所使用到的纳米晶/非晶复合CuZrAg粉是用物理方法制备得到,即使用激光加热金属靶材使金属元素汽化,相比于通过改性银粉从而提高其导电性的方法,这种物理添加方法的制备工艺简单,省略了繁琐的化学反应流程,更避开了很多化学法制备纳米金属颗粒时用到的危险化学品,本发明的安全系数远远高于大部分化学改性方法;
(2)相比于现有的导电银浆工艺,本发明的操作流程简单,纳米晶/非晶复合CuZrAg粉生产效率高,只需简单添加即可;
(3)本发明所用到的纳米晶/非晶复合CuZrAg粉中Ag的占比仅为17.5%,Cu和Zr相比于Ag都是价格更低的原材料,从而使得整体银浆的成本下降,考虑到增加此种纳米晶/非晶复合CuZrAg粉获得的巨大的导电性的提高以及成本的降低,其高性能迎合市场需求,高性价比符合市场规律,具有广泛的商业前景。
附图说明
图1为高真空制粉腔室示意图。
图2为纳米晶/非晶复合CuZrAg粉透射电子显微镜图。
图3为纳米晶/非晶复合CuZrAg粉选区电子衍射图。
图4为对比例1中未添加纳米晶/非晶复合CuZrAg粉的导电银浆网络扫描电镜图。
图5为实施例3纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的导电银浆网络扫描电镜图。
具体实施方式
下面结合数据对本发明做进一步描述,具体实施方式不限于此。本发明主要提供不同分数的CuZrAg浆料对商用导电银浆的改性结果,因此在进行实施例之前先要进行纳米晶/非晶复合CuZrAg粉的制备,操作步骤如发明内容所述。下面介绍具体实施例。
结合图1,本发明提供了一种用于处理容器装置:包含一高真空制粉腔室,包含一个外置激光发射器,用于激发金属靶材中的原子。包含一个液氮冷却罐,用于对腔体中金属纳米颗粒的吸附沉积;包含一个方柱形收粉罐置于液氮冷却罐的下方,用于收集冷却罐上刮落的金属纳米颗粒;包含一组机械泵和分子泵,用于保证腔室内的超高真空度。
对比例1
不含纳米晶/非晶复合CuZrAg粉导电银浆的制备。
其各组分所占总浆料的质量分数为:银粉58、分散剂BYK0.5、玻璃粉1、载体40.5,载体的配比为:松油醇40、丁基卡必醇35.4、丁基卡必醇醋酸酯8、醇酯十二8、乙基纤维素6.6、司班85 2,混合搅拌24小时后得到不含纳米晶/非晶复合CuZrAg粉导电银浆。
采用丝网印刷机将得到的导电银浆刷于20mm×10mm的Si基板上,自然平流10min,在200℃下干燥15min,然后在800℃下保温1min快速烧结成膜。使用四探针电阻仪测得其方阻为8.7mΩ/□。
实施例1
5g含0.5%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的制备。
其各组分所占总浆料的质量分数为:银粉57.5、纳米晶/非晶复合Cu47.5Zr35Ag17.5粉0.5、分散剂BYK0.5、玻璃粉1、载体40.5,载体由以下质量份的原料配成:松油醇40、丁基卡必醇35.4、丁基卡必醇醋酸酯8、醇酯十二8、乙基纤维素6.6、司班85 2。
步骤1:将CuZrAg靶材(原子比为47.5:35:17.5)进行表面预处理,打磨,抛光去除表面氧化层,用酒精超声清洗后,固定在高真空制粉腔体内相应位置。
步骤2:将腔室密封,通过机械泵和分子泵将制粉腔内气压抽至超高真空状态(低于10-6Pa),待真空稳定后,向制粉腔内缓慢输入800Pa的高纯氦气。
步骤3:向液氮冷却罐中输入液氮,直至液氮罐充满液氮。
步骤4:将外置激光器瞄准腔体内的金属靶材,调整激光角度使发射出的激光垂直于靶材,同时调整激光器距离靶材的距离,使得激光发射镜头到靶材的距离在70-80cm之间。以保证激光打到靶材上的功率是最大功率。金属靶表面蒸发出的金属蒸汽或金属原子和腔室中的惰性气体氦气发生碰撞并快速降温,形成新的固相纳米粉末,由于液氮罐内超低温液氮的原因,吸附并沉积在液氮罐外侧铜辊表面。
步骤5:转动铜辊旁的刮刀,将铜辊上的纳米晶/非晶复合CuZrAg粉刮落至下方的方柱形收粉罐中。
步骤6:按微米银粉57.5份、纳米晶/非晶复合CuZrAg粉0.5份,分散剂BYK0.5、玻璃粉1、载体40.5,载体的配比为:松油醇40、丁基卡必醇35.4、丁基卡必醇醋酸酯8、醇酯十二8、乙基纤维素6.6、司班85 2的配方配制5g复合导电银浆,搅拌24小时;得到含有0.5%纳米晶/非晶复合CuZrAg粉的复合导电银浆。
方阻测试方法同实施例1,测得含0.5%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的方阻为7.03mΩ/□。
实施例2
5g含1%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的制备方法同实施例1,其中微米银粉质量份57份,纳米晶/非晶复合Cu47.5Zr35Ag17.5粉质量份1份
方阻测试方法同实施例1,测得含0.5%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的方阻为5.63mΩ/□。
实施例3
5g含2%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的制备方法同实施例1,其中微米银粉质量份56份,纳米晶/非晶复合Cu47.5Zr35Ag17.5粉质量份2份。
方阻测试方法同实施例1,测得含0.2%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的方阻为6.89mΩ/□。
实施例4
5g含1%纳米晶/非晶复合Cu47.5Zr25Ag27.5粉的复合导电银浆的制备方法同实施例1,其中微米银粉质量份57份,纳米晶/非晶复合Cu47.5Zr35Ag17.5粉质量份1份。
方阻测试方法同实施例1,测得含0.1%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的复合导电银浆的方阻为5.10mΩ/□。
高温烧结后制成的电极表面银白,光滑无缺陷,浆料附着力好。除实施例以外,我们还制备了其他添加不同含量以及不同铜锆银成份的纳米晶/非晶铜锆银粉的复合导电银浆并测试其方阻,具体方阻变化规律如表1所示。
表1
方阻/mΩ/□ | 0% | 0.5% | 0.75% | 1% | 1.5% | 2% | 3% | 5% |
Cu<sub>47.5</sub>Zr<sub>35</sub>Ag<sub>17.5</sub> | 8.7 | 7.03 | 6.47 | 5.63 | 6.32 | 6.89 | 8.02 | 8.86 |
Cu<sub>47.5</sub>Zr<sub>30</sub>Ag<sub>22.5</sub> | 8.7 | 6.85 | 6.39 | 5.34 | 6.21 | 6.65 | 7.82 | 8.81 |
Cu<sub>47.5</sub>Zr<sub>25</sub>Ag<sub>27.5</sub> | 8.7 | 6.77 | 6.21 | 5.10 | 6.09 | 6.57 | 7.59 | 8.60 |
通过采用上述技术方案,导电银浆的成本略微降低,而导电性能得到了极大的提高,烘烤后的导电银浆网络也得到了非常好的改善。未添加纳米晶/非晶复合CuZrAg粉的导电银浆网络如图4所示,添加1%纳米晶/非晶复合Cu47.5Zr35Ag17.5粉的导电银浆网络图5所示。
Claims (7)
1.一种含纳米晶/非晶复合CuZrAg粉的复合导电银浆,其特征在于,由以下重量份的原料制得:
微米银粉53-58份、纳米晶/非晶复合CuZrAg粉0.5-5份,分散剂BYK0.5份、玻璃粉1份、载体40.5份,载体的配比为:松油醇40份、丁基卡必醇35.4份、丁基卡必醇醋酸酯8份、醇酯十二8份、乙基纤维素6.6份、司班85 2份。
2.一种用于制备复合导电银浆容器装置,其特征在于,该装置包含一高真空制粉腔室,包含一个外置激光发射器,用于激发金属靶材中的原子;包含一个液氮冷却罐,用于对腔体中金属纳米颗粒的吸附沉积;包含一个方柱形收粉罐置于液氮冷却罐的下方,用于收集冷却罐上刮落的金属纳米颗粒;包含一组机械泵和分子泵,用于保证腔室内的超高真空度。
3.一种含纳米晶/非晶复合CuZrAg粉制备方法,其特征在于,该方法具体为
将CuZrAg靶材进行表面预处理,打磨,抛光去除表面氧化层,用酒精超声清洗后,固定在高真空制粉腔体内相应位置;
将腔室密封,通过机械泵和分子泵将制粉腔内气压抽至超高真空状态,待真空稳定后,向制粉腔内缓慢输入800Pa的高纯氦气;
向液氮冷却罐中输入液氮,直至液氮罐充满液氮;
将外置激光器瞄准腔体内的金属靶材,调整激光角度使发射出的激光垂直于靶材,同时调整激光器距离靶材的距离;
转动铜辊旁的刮刀,将铜辊上的纳米晶/非晶复合CuZrAg粉刮落至下方的方柱形收粉罐中;
按配方混合,搅拌24小时;得到含有纳米晶/非晶复合CuZrAg粉的复合导电银浆。
4.根据权利要求3所述的制备方法,其特征在于,超高真空状态为低于10-6Pa。
5.根据权利要求3所述的制备方法,其特征在于,使得激光发射镜头到靶材的距离在70-80cm之间。
6.根据权利要求3所述的制备方法,其特征在于,配方为微米银粉53-58份、纳米晶/非晶复合CuZrAg粉0.5-5份,分散剂BYK0.5份、玻璃粉1份、载体40.5份,载体的配比为:松油醇40份、丁基卡必醇35.4份、丁基卡必醇醋酸酯8份、醇酯十二8份、乙基纤维素6.6份、司班852份。
7.根据权利要求3所述的制备方法,其特征在于,CuZrAg靶材为市购。
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