CN107460460B - 一种制备自支撑三维多孔铜薄膜的方法及自支撑铜薄膜 - Google Patents

一种制备自支撑三维多孔铜薄膜的方法及自支撑铜薄膜 Download PDF

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CN107460460B
CN107460460B CN201710562980.8A CN201710562980A CN107460460B CN 107460460 B CN107460460 B CN 107460460B CN 201710562980 A CN201710562980 A CN 201710562980A CN 107460460 B CN107460460 B CN 107460460B
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樊小勇
倪珂帆
韩家兴
王珊
苟蕾
李东林
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Abstract

本发明提出一种制备自支撑三维多孔铜薄膜的方法，包括以下步骤：将玻璃薄膜或塑料薄膜在敏化液中进行敏化，随后在活化液中进行活化，所述活化液包括氯化钯和盐酸的混合液；经活化后的玻璃薄膜或塑料薄膜放入混合溶液中浸泡得到前驱体，所述混合溶液包括柠檬酸三钠、硫酸镍、硫酸铜、硼酸、次亚磷酸钠、2,4,7,9‑四甲基‑5‑癸炔‑4,7‑二醇、十六烷基三甲基溴化铵和聚乙二醇的混合液；将前驱体加热到使前驱体中的玻璃薄膜脱离，或者将前驱体中的塑料薄膜用有机溶剂溶掉，获得自支撑三维多孔铜薄膜。本发明的制备方法，相对于模板法、去合金法和电沉积法等工艺，极大简化了制备步骤，只简单采用敏化、活化及浸泡即可实现。

Description

一种制备自支撑三维多孔铜薄膜的方法及自支撑铜薄膜
技术领域
本发明属于三维多孔金属薄膜制备技术领域，涉及三维多孔铜薄膜，具体涉及一种自支撑三维多孔铜薄膜的制备方法及由该方法制备出的自支撑铜薄膜。
背景技术
三维多孔金属电极具有较大的比表面积和贯通的结构,有利于电极与气相或液相介质的充分接触和电子传递,在燃料电池、电化学电容器和电化学传感器等领域都有广泛的应用。
目前制备铜薄膜往往采用模板法和合金的选择性电化学溶出法等，这些方法均很复杂，并且制备出的铜薄膜含有不同的基底，这些基底的存在无形中提高了电极材料的内阻，不利于铜薄膜电化学性能的充分发挥。
发明内容
针对现有技术存在的不足，本发明的目的在于，提供一种自支撑三维多孔铜薄膜的制备方法及由该方法制备出的自支撑铜薄膜，制备方法简单，自支撑的铜薄膜无基底。
为了解决上述技术问题，本发明采用如下技术方案予以实现：
一种制备自支撑三维多孔铜薄膜的方法，包括以下步骤：
将玻璃薄膜或塑料薄膜在敏化液中进行敏化，所述敏化液包括氯化亚锡和盐酸的混合液；
将敏化后的玻璃薄膜或塑料薄膜在活化液中进行活化，所述活化液包括氯化钯和盐酸的混合液；
经活化后的玻璃薄膜或塑料薄膜放入混合溶液中浸泡得到前驱体，所述混合溶液包括柠檬酸三钠、硫酸镍、硫酸铜、硼酸、次亚磷酸钠、2,4,7,9-四甲基-5-癸炔-4,7-二醇、十六烷基三甲基溴化铵和聚乙二醇的混合液；
将前驱体加热到使前驱体中的玻璃薄膜脱离，或者将前驱体中的塑料薄膜用有机溶剂溶掉，获得自支撑三维多孔铜薄膜。
前述步骤中，优选的，将前驱体加热到500℃时前驱体中的玻璃薄膜脱离。
本发明的有机溶剂可选用丙酮或者四氢呋喃。
本发明的混合溶液pH为8～11。
所述敏化液的制备包括将氯化亚锡和盐酸溶于去离子水中，氯化亚锡的质量浓度为20g/L，盐酸摩尔浓度为1mol/L，敏化时间为15-20min。
所述活化液的制备包括将氯化钯和盐酸分别溶于去离子水中，活化液中氯化钯的质量浓度为0.8g/L，盐酸摩尔浓度1mol/L，活化时间为3-5min。
所述混合溶液中柠檬酸三钠的质量浓度为5g/L～20g/L，硫酸镍的质量浓度为0.1g/L～1g/L，硫酸铜的质量浓度为5g/L～15g/L，硼酸的质量浓度为5g/L～35g/L，次亚磷酸钠的质量浓度为5g/L～30g/L，2,4,7,9-四甲基-5-癸炔-4,7-二醇的质量浓度为0.1g/L～10g/L，十六烷基三甲基溴化铵的质量浓度为0.1g/L～10g/L，聚乙二醇的质量浓度为0.1g/L～10g/L。
所述浸泡时间为15min～90min，浸泡水浴温度为40℃～60℃。
敏化前将玻璃薄膜或塑料薄膜进行粗化清洗处理。
一种按照上述方法制备的自支撑三维多孔铜薄膜，该自支撑铜薄膜无基底，具有三维呈圆形贯穿孔，孔径分布为1μm-15μm。
本发明与现有技术相比，具有如下技术效果：
1)本发明的制备方法，相对于模板法、去合金法和电沉积法等工艺，极大简化了制备步骤，只简单采用敏化、活化及浸泡即可实现。
2)采用本方法制备出的三维多孔铜薄膜结构中不含基底。
3)采用该方法制备出的三维多孔铜薄膜的孔径在1-15μm范围可调，对锂离子电池和钠离子电池电极材料充放电过程中体积变化具有很好的缓解作用。传统泡沫镍或泡沫铜的孔径在0.5mm左右；电沉积法制备的三维多孔金属孔径也在0.5mm左右；这两种方法对锂离子电池和钠离子电池电极材料充放电过程中体积变化缓解作用较差。
4)采用该方法制备出的三维多孔铜薄膜具有三维贯穿圆形孔，且孔径分布均匀，有利于离子快速传输。目前采用去合金法制备的三维多孔金属主要为狭窄孔，且不贯穿孔，降低了离子传输速率。
以下结合实施例对本发明的具体内容作进一步详细解释说明。
附图说明
图1为自支撑三维多孔铜薄膜的宏观照片。
图2为实施例1的SEM图。
图3为实施例2的SEM图。
图4为实施例3的SEM图。
图5为对比例1的SEM图。
具体实施方式
以下仅以各原料的取值范围中的某个值举例给出本发明的具体实施例，需要说明的是本发明并不局限于以下具体实施例，应当理解涵盖以上的取值范围，并且凡在本申请技术方案基础上做的等同变换均落入本发明的保护范围。
本发明制备的前驱体为在玻璃或塑料薄膜上长出一层三维多孔铜薄膜，之后经去基底，获得无基底存在的自支撑三维多孔铜薄膜，见附图1。
实施例1：
本实施例给出一种制备自支撑三维多孔铜薄膜的方法，包括以下步骤：
(1)将玻璃片粗化后放在在丙酮溶液中超声清洗2min，再放入0.1mol/L盐酸中清洗30s，之后放入含有20g/L的氯化亚锡，1mol/L盐酸的溶液中敏化15min。
(2)将敏化后的玻璃片在含有0.8g/L氯化钯和1mol/L盐酸溶液中活化5min。
(3)配置混合溶液，包含5g/L柠檬酸三钠，5g/L硫酸铜，0.1g/L硫酸镍，5g/L硼酸，5g/L次亚磷酸钠，0.1g/L 2,4,7,9-四甲基-5-癸炔-4,7-二醇，0.1g/L聚乙二醇，0.1g/L十六烷基三甲基溴化铵。采用NaOH溶液调节混合镍溶液pH值为8。将配制的混合溶液放入40℃恒温水浴锅中，浸泡15分钟后清洗，在Ar气氛下加热到500℃，得到无基底的自支撑三维多孔铜薄膜。该自支撑三维多孔铜薄膜的孔径为1-5微米，孔分布不均匀，见附图2。
将实施例1制备得到的铜薄膜经冷冻干燥处理后，剪成2cm×0.5cm的长条，在其两端粘着银胶，粘上铜线作为电极，再将其嵌入旋涂好的PDMS中，并在上层覆盖一层PDMS，静置抽真空后经干燥保湿即得到简易应变传感器，实验结果显示，应变传感器的导电性能提高。
实施例2：
本实施例给出一种制备自支撑三维多孔铜薄膜的方法，与实施例1相同，不同的是，基底用塑料薄膜，步骤(3)中溶液含10.0g/L柠檬酸三钠，8g/L硫酸铜，1.5g/L硫酸镍，20g/L次亚磷酸钠，30g/L硼酸，5g/L 2,4,7,9-四甲基-5-癸炔-4,7-二醇，5g/L聚乙二醇，5g/L十六烷基三甲基溴化铵。用NaOH溶液调节pH为11，40℃恒温水浴中，化学镀60分钟，清洗后，丙酮清洗，得到无基底的自支撑三维多孔铜薄膜。用量不同导致该自支撑三维多孔铜薄膜的孔径为1-10微米，孔分布均匀，见附图3。
实施例3：
本实施例给出一种制备自支撑三维多孔铜薄膜的方法，与实施例1相同，不同的是，步骤(3)中，溶液含20g/L柠檬酸三钠，15g/L硫酸铜，1g/L硫酸镍，35g/L硼酸，30g/L次亚磷酸钠，10g/L 2,4,7,9-四甲基-5-癸炔-4,7-二醇，10g/L聚乙二醇，10g/L十六烷基三甲基溴化铵。用NaOH溶液调节pH为11，60℃恒温水浴中，化学镀90分钟，清洗后，在Ar气氛下加热到500℃，得到无基底的自支撑三维多孔铜薄膜。该自支撑三维多孔铜薄膜的孔径为1-15微米，孔分布均匀，见附图4。
对比例1：
本对比例给出一种制备三维多孔铜薄膜的方法，与实施例2相同，不同的是，用NaOH溶液调节混合溶液pH为14，80℃恒温水浴中，化学镀90分钟，清洗后，在Ar气氛下加热到500℃，得到三维多孔铜薄膜。该三维多孔铜薄膜的孔径为1-5微米，但是孔结构出现坍塌，自支撑结构无法实现，见附图5。
实施例4：
本实施例给出一种制备自支撑三维多孔铜薄膜的方法，与实施例1相同，不同的是，步骤(1)中采用塑料薄膜为基底。去基底时，在丙酮溶液中浸泡24小时，获得无基底的自支撑三维多孔铜薄膜。孔结构与实施例1相似。

Claims (8)

1.一种制备自支撑三维多孔铜薄膜的方法，其特征在于，包括以下步骤：
将玻璃薄膜或塑料薄膜在敏化液中进行敏化，所述敏化液包括氯化亚锡和盐酸的混合液；
将敏化后的玻璃薄膜或塑料薄膜在活化液中进行活化，所述活化液包括氯化钯和盐酸的混合液；
经活化后的玻璃薄膜或塑料薄膜放入混合溶液中浸泡得到前驱体，所述混合溶液包括柠檬酸三钠、硫酸镍、硫酸铜、硼酸、次亚磷酸钠、2,4,7,9-四甲基-5-癸炔-4,7-二醇、十六烷基三甲基溴化铵和聚乙二醇的混合液；所述混合溶液pH值为8～11；所述混合溶液中柠檬酸三钠的质量浓度为5g/L～20g/L，硫酸镍的质量浓度为0.1g/L～1g/L，硫酸铜的质量浓度为5g/L～15g/L，硼酸的质量浓度为5g/L～35g/L，次亚磷酸钠的质量浓度为5g/L～30g/L，2,4,7,9-四甲基-5-癸炔-4,7-二醇的质量浓度为0.1g/L～10g/L，十六烷基三甲基溴化铵的质量浓度为0.1g/L～10g/L，聚乙二醇的质量浓度为0.1g/L～10g/L；
将前驱体中的玻璃薄膜或塑料薄膜进行脱模获得自支撑三维多孔铜薄膜；所述脱模包括将前驱体加热到使前驱体中的玻璃薄膜脱离，或者用有机溶剂溶去前驱体中的塑料薄膜。
2.如权利要求1所述方法，其特征在于，将前驱体加热到500℃使前驱体中的玻璃薄膜脱离。
3.如权利要求1所述方法，其特征在于，所述有机溶剂包括丙酮和四氢呋喃。
4.如权利要求1所述方法，其特征在于，所述敏化液的制备包括将氯化亚锡和盐酸溶于去离子水中，氯化亚锡的质量浓度为20g/L，盐酸摩尔浓度为1mol/L，敏化时间为15min～20min。
5.如权利要求1所述方法，其特征在于，所述活化液的制备包括将氯化钯和盐酸分别溶于去离子水中，活化液中氯化钯的质量浓度为0.8g/L，盐酸摩尔浓度为1mol/L，活化时间为3min～5min。
6.如权利要求1所述方法，其特征在于，所述浸泡时间为15min～90min，浸泡温度为40℃～60℃。
7.如权利要求1所述方法，其特征在于，敏化前将玻璃薄膜或塑料薄膜进行粗化清洗处理。
8.一种按照权利要求1所述方法制备的自支撑三维多孔铜薄膜，其特征在于：所述自支撑三维多孔铜薄膜无基底，孔呈圆形贯穿孔，孔径分布为1μm～15μm。
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