CN110238386A - 超细立方单晶银粉的制备方法 - Google Patents
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Abstract
本发明公开了一种超细立方单晶银粉的制备方法，包括以下步骤：(1)将乙二醇加热至170℃，保持170℃的温度加入NaBr、NaCl和聚乙烯吡咯烷酮搅拌均匀得到溶液Ⅰ；(2)继续保持溶液Ⅰ在170℃的温度下注射加入AgNO3溶液，注射加入AgNO3溶液的过程保持对溶液Ⅰ的搅拌，在此条件下AgNO3与乙二醇发生反应，AgNO3中的Ag+被还原得到立方状态的银，此时溶液Ⅰ变成溶液Ⅱ。本发明的超细立方单晶银粉的制备方法，在170℃的温度下，采用聚乙烯吡咯烷酮作为分散剂，同时配合NaBr、NaCl，三者的协同作用共同作用使得制备的银粉成为立方状的颗粒，制得的颗粒均匀而且分散度好。制备方法简单，便于操作。
Description
技术领域
本发明涉及银粉制备方法技术领域，特别涉及一种超细立方单晶银粉的制备方法。
背景技术
当功能性材料超细化后，粒径处于微米、亚微米和纳米尺寸时，其尺度介于原子、分子与块状材料之间，物理化学性质都有很大的变化，被称之为物质的第四状态。随着物质的超细化，其表面分子排列与电子排列分布结构以及晶体结构都发生相应的变化，产生了块状材料所不具有的奇特的小尺寸效应、表面效应、宏观量子隧道效应与量子尺寸效应，进而使得超细粉体与一般大体积材料相比，在物理、化学以及界面方面都有更优异的性质，从而在应用方面有意想不到的效果。
超细银粉为微米级粒度的银粉，其颗粒形态有球状、絮状、树枝状、棒状、线状、立方状、片状和微晶。超细银粉的粒径小、比表面积大。这种结构使其熔点岁随颗粒变小而降低，超细银粉表面原子的原子间相互作用及电子能谱同银粉内部均有不同，具有很大的化学活性，因此，在其使用于电子元器件上时，与表面有关的吸附、催化、扩散、烧结等特性明显与大粒径的银粉末有显著不同，有良好的导电性能。另外，超细功能的体积效应(即体积缩小，粒子内的原子数目减少而引起的效应)使得能带点的能级间隔加大，其质子振动和能级均不连续。活性强，易于进行各种化学反应，有很强的的吸附能力和催化活性。超细粒子的表面有许多悬空键，具有不饱和性质，从而导致超细银粉的特殊吸附现象和催化性质。
超细银粉的制备方法包括气相法、固相法和液相法。气相法的投资大、能耗高、产率低；固相法制备的银粉粒径偏大而且粒径分布范围宽；液相法工艺过程比较简单，粉体颗粒大小和形状容易控制，是目前低成本制备银粉常用的方法。现有技术中有很多采用液相法制备超细银粉的方法，主要采用还原剂如葡萄糖、水合肼、硼氰化钠、抗坏血酸等在液相中还原银盐溶液得到超细银粉，制得的银粉有球状、树枝状等，但是现有技术中液相法制备的超细银粉分散度差，还没有采用化学方法制备超细立方单晶银粉的报道，例如申请号为2015107269865的树叶状银粉的制备方法。
发明内容
有鉴于此，本发明的目的在于提供一种采用液相还原法制备超细立方单晶银粉的方法，制得的银粉分散性好，而且粒径分布均匀。具体而言通过以下技术方案实现：
本发明的超细立方单晶银粉的制备方法，包括以下步骤：
(1)将乙二醇加热至170℃，保持170℃的温度加入NaBr、NaCl和聚乙烯吡咯烷酮搅拌均匀得到溶液Ⅰ；
(2)继续保持溶液Ⅰ在170℃的温度下注射加入AgNO3溶液，注射加入AgNO3溶液的过程保持对溶液Ⅰ的搅拌，在此条件下AgNO3与乙二醇发生反应，AgNO3中的Ag+被还原得到立方状态的银，此时溶液Ⅰ变成溶液Ⅱ。
进一步，还包括步骤(3)：对于步骤(2)得到立方状态的银后，所述溶液Ⅱ在25℃下冷却反应，然后缓慢加入丙酮，然后在6000rpm下离心10分钟，用乙醇清洗除去杂质。先冷却再加入丙酮，防止丙酮被氧化
进一步，所述步骤(1)采用沙浴对乙二醇加热并保持温度。
进一步，所述步骤(2)中注射加入AgNO3的注射速率为5ml/h。
进一步，所述NaBr、NaCl、聚乙烯吡咯烷酮和AgNO3的质量比为71：71：1000：532。
本发明的有益效果：本发明的超细立方单晶银粉的制备方法，在170℃的温度下，采用聚乙烯吡咯烷酮作为分散剂，同时配合NaBr、NaCl，三者的协同作用共同作用使得制备的银粉成为立方状的颗粒，制得的颗粒均匀而且分散度好。制备方法简单，便于操作。
附图说明
下面结合附图和实施例对本发明作进一步描述：
图1和图2为采用本发明方法制得的超细立方单晶银粉的电镜扫描图。
具体实施方式
本实施例中的超细立方单晶银粉的制备方法，首先将40ml的乙二醇在170℃的沙浴中加热20min加热至170℃，然后在保持170℃温度并搅拌的条件下加入14.2mgNaBr、14.2mgNaCl和聚乙烯吡咯烷酮(polyvinyl pyrrolidone，简称PVP，采用平均相对分子质量为130000的聚乙烯吡咯烷酮)，搅拌30min得到溶液Ⅰ。取106.4mg分析纯的固体AgNO3溶入1ml水中形成AgNO3溶液，继续保持170℃温度并搅拌的条件下在用注射泵向溶液中注射配制的AgNO3溶液，注射速率为5ml/h，在此条件下AgNO3与乙二醇发生反应，AgNO3中的Ag+被还原得到立方状态的银，此时溶液Ⅰ变成溶液Ⅱ。得到立方状态的银后，溶液Ⅱ在25℃下冷却反应，然后缓慢加入丙酮2ml，然后在6000rpm下离心10分钟，用乙醇清洗除去杂质,重复清洗直到清洗干净为止。
液相还原制备银粉过程中，需要克服制备出来的颗粒之间的团聚问题。粉体的团聚主要存在于两个过程中，其一是在还原过程中，首先还原出来的超细颗粒由于搅拌热运动等因素互相碰撞团聚在一起。本发明中采用聚乙烯吡咯烷酮作为分散剂，同时配合NaBr、NaCl，三者的协同作用共同作用使得制备的银粉成为立方状的颗粒，制得的颗粒均匀而且分散度好，如图1和图2所示，制得的银粉为立方状，粒度均匀并且分散度好。
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。
Claims (5)
1.一种超细立方单晶银粉的制备方法，其特征在于包括以下步骤：
(1)将乙二醇加热至170℃，保持170℃的温度加入NaBr、NaCl和聚乙烯吡咯烷酮搅拌均匀得到溶液Ⅰ；
(2)继续保持溶液Ⅰ在170℃的温度下注射加入AgNO3溶液，注射加入AgNO3溶液的过程保持对溶液Ⅰ的搅拌，在此条件下AgNO3与乙二醇发生反应，AgNO3中的Ag+被还原得到立方状态的银，此时溶液Ⅰ变成溶液Ⅱ。
2.根据权利要求1所述的超细立方单晶银粉的制备方法，其特征在于还包括步骤(3)：对于步骤(2)得到立方状态的银后，所述溶液Ⅱ在25℃下冷却反应，然后缓慢加入丙酮，然后在6000rpm下离心10分钟，用乙醇清洗除去杂质。
3.根据权利要求1所述的超细立方单晶银粉的制备方法，其特征在于：所述步骤(1)采用沙浴对乙二醇加热并保持温度。
4.根据权利要求1所述的超细立方单晶银粉的制备方法，其特征在于：所述步骤(2)中注射加入AgNO3的注射速率为5ml/h。
5.根据权利要求1所述的超细立方单晶银粉的制备方法，其特征在于：所述NaBr、NaCl、聚乙烯吡咯烷酮和AgNO3的质量比为71：71：1000：532。
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| CN111570822A (zh) * | 2020-06-29 | 2020-08-25 | 河南金渠银通金属材料有限公司 | 一种纳米银粉及其制备方法 |
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