CN109305806A - 一种三维多孔材料的制备方法 - Google Patents

一种三维多孔材料的制备方法 Download PDF

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CN109305806A
CN109305806A CN201811320957.9A CN201811320957A CN109305806A CN 109305806 A CN109305806 A CN 109305806A CN 201811320957 A CN201811320957 A CN 201811320957A CN 109305806 A CN109305806 A CN 109305806A
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邵国胜
张鹏
苗富军
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Zhengzhou New Century Material And Genome Engineering Research Institute Co Ltd
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Abstract

本发明属于材料制备技术领域，具体涉及一种三维多孔材料的制备方法。本发明的制备方法包括以下步骤：（1）将前驱体、PAN、PVP和DMF混合均匀，得混合液A；所述前驱体为硅源、铜源、钛源、镍源、锌源中的一种或几种的组合；（2）将混合液A均匀填充到模具中，然后将模具浸入到碱性溶液中，保持0.5h，得多孔薄膜，然后煅烧得三维多孔材料。本发明的制备方法成功构筑了一系列三维多孔材料，并且实现了孔结构的精细调控。本发明的制备方法具有普适性，并且工艺简单、流程短、设备依赖性低，适用于工业化大规模生产。

Description

一种三维多孔材料的制备方法
技术领域
本发明属于材料制备技术领域，具体涉及一种三维多孔材料的制备方法。
背景技术
多孔材料由于其多孔结构具有高孔隙率、高透过性、高吸附性和高组装性等优异的物理化学性能，具有广阔的应用前景尤其是在储能以及催化领域。目前模板法是合成多孔材料的一种重要方法。模板法的最大优点在于基体反相复制模板结构，通过改变模板剂的结构和用量可以有效调节产物的孔结构。双模板（软硬模板）法也是目前常见的制备方式，通过调控相关参数实现不同织构的分级孔结构材料制备。然而目前采用的模板剂不仅价格昂贵，还很容易造成环境污染，特别是模板法必须经历一系列模板去除以形成分级孔结构的后处理步骤，以上这些都严重的限制了模板法在多孔材料制备领域的发展。
东北师范大学的苗富军的博士论文《三维多孔碳基纳米材料的制备及其电化学性质研究》公开了一种三维多孔碳薄膜材料的制备方法，该方法利用复合纤维PAN不溶于水，PVP和DMF溶于水的性质，采用高浓度PAN/PVP/DMF前驱体溶液通过浸渍沉降相分离方法和高温碳化处理，制备了自支撑多孔碳薄膜材料。但是该文中没有涉及含氧化物的三维多孔材料的制备。
发明内容
本发明的目的在于提供一种三维多孔材料的制备方法，可用于制备含氧化物的三维多孔材料。
为实现上述目的，本发明所采用的技术方案为：
一种三维多孔材料的制备方法，包括以下步骤：
（1）将前驱体、PAN、PVP和DMF混合均匀，得混合液A；所述前驱体为硅源、铜源、钛源、镍源、锌源中的一种或几种的组合；
（2）将混合液A均匀填充到模具中，然后将模具浸入到碱性溶液中，保持0.5h，得多孔薄膜，然后煅烧得三维多孔材料。
本发明的制备方法过程中，使用不同的前驱体可直接得到不同的含氧化物三维多孔材料，具有普适性。本发明的制备方法中PAN不溶于水，PVP和DMF溶于水，三者组成了三元相分离溶液，然后加入可以与碱性溶液发生水解的前驱体，利用碱性溶液浸渍产生相分离原理与高温烧结相结合，制备了三维多孔氧化物材料。在本发明的制备方法中，PVP和DMF溶于水从而在煅烧前形成了多孔薄膜，通过控制二者的量即可控制孔径的大小。本发明的制备方法具有工艺简单、流程短、高效、设备依赖性低、适用于工业化大规模生产。
采用碱性溶液可促进前驱体水解，在可溶性组分PVP和DMF的溶解过程中尽可能保留在多孔PAN骨架中。本发明的制备方法制得的三维多孔材料具有良好的三维连通多孔结构，较高的孔隙率、高孔堆积密度以及三维交联骨架网络结构。这种三维多孔结构能够促进溶液在材料内部快速扩散，高的比表面积为离子提供更多的活性位点，促进更多离子吸附，可应用于催化、储能、传感、分离等领域。此外，高度交联的三维骨架结构能够保证材料的物理稳定性。按照此方法制备的三维多孔材料可作为活性模板进行其它功能材料复合，并应用于相关领域。
为实现均匀三维多孔骨架的构建，步骤（1）所述PAN和PVP在混合液A中的总质量分数不低于20%。
步骤（1）所述前驱体在混合液A中的质量分数不低于3%。
步骤（2）所述煅烧为在有氧气氛下，将多孔薄膜在500~700℃温度下保温1~4h。在有氧气氛下可将多孔PAN骨架烧掉，得到氧化物多孔材料。
步骤（2）所述煅烧为在惰性气氛下，将多孔薄膜在500~700℃温度下保温1~4h。在惰性气氛下煅烧，可将多孔PAN骨架转化为多孔碳，从而得含氧化物的三维多孔碳复合材料。
煅烧过程中升温速率为1~5℃/min，相对较慢的升温速率能够防止多孔薄膜结构在热处理过程中的快速收缩，从而保证微结构的完整。
附图说明
图1为本发明的制备三维多孔材料的工艺流程图；
图2为本发明的实施例1制备的三维多孔氧化硅材料的微观SEM图；
图3为本发明的实施例14制备的三维多孔氧化铜材料的微观SEM图；
图4为本发明的实施例15制备的三维多孔氧化钛材料的微观SEM图；
图5为本发明的实施例16制备的三维多孔氧化镍材料的微观SEM图；
图6为本发明的实施例17制备的三维多孔氧化锌材料的微观SEM图；
图7为本发明的实施例18制备的三维多孔碳复合材料的微观SEM图。
具体实施方式
本发明所用前驱体为溶于且稳定的存在于PAN/PVP/DMF高分子溶液中的化合物。
本发明的三维多孔材料的制备过程中所用硅源为TEOS。
本发明的三维多孔材料的制备过程中所用铜源为醋酸铜、硝酸铜、氯化铜中的一种。
本发明的三维多孔材料的制备过程中所用钛源为四氯化钛、异丙醇钛中的一种。
本发明的三维多孔材料的制备过程中所用镍源为醋酸镍、硝酸镍、氯化镍中的一种。
本发明的三维多孔材料的制备过程中所用锌源为硝酸锌、醋酸锌、氯化锌中的一种。
本发明的三维多孔材料的制备流程如图1所示，干燥后得到的多孔薄膜通过煅烧即可得到三维多孔材料。
下面结合具体实施例对本发明的三维多孔材料的制备方法作进一步说明，以下实施例中所用试剂均为市售。
实施例1
本实施例的三维多孔氧化硅材料的制备方法，包括以下步骤：
（1）将1mL TEOS，2gPAN和2gPVP依次溶于10mLDMF溶液中，搅拌至溶液澄清，得到含有硅的前驱体溶液；
（2）将含有硅的前驱体溶液倒入石英凹槽（尺寸为长度*宽度*深度：70mm * 30mm *1mm）中，采用刮涂的方式，使得溶液均匀填充在石英凹槽中；
（3）将石英凹槽浸入到0.1M氢氧化钠水溶液中，保持0.5h，使得可溶性组分PVP和DMF充分溶解到水溶液中，得到不溶性组分PAN形成的多孔薄膜，并与石英凹槽分离；
（4）将多孔薄膜取出，用去离子水冲洗然后在通风处晾干，然后将晾干后的薄膜置于管式炉中在空气气氛下，从室温以3℃/min的升温速率升到700℃，并保温2h，得三维多孔氧化硅材料。
根据图2所示，本实施例制得的三维多孔氧化硅材料的孔径大小约为150nm，具有交联的三维骨架网络，具有相连通的孔结构。
实施例2
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中TEOS的体积为0.5mL，其他均相同。
实施例3
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中TEOS的体积为2mL，其他均相同。
实施例4
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中PAN的质量为1g，其他均相同。
实施例5
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中PAN的质量为1.5g，其他均相同。
实施例6
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中PVP的质量为1g，其他均相同。
实施例7
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（1）中PVP的质量为1.5g，其他均相同。
实施例8
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中煅烧温度为500℃，其他均相同。
实施例9
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中煅烧温度为600℃，其他均相同。
实施例10
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中升温速率为1℃/min，其他均相同。
实施例11
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中升温速率为5℃/min，其他均相同。
实施例12
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中保温时间为1h，其他均相同。
实施例13
本实施例的三维多孔材料的制备方法与实施例1不同的是步骤（4）中保温时间为4h，其他均相同。
实施例14
本实施例的三维多孔材料的制备方法与实施例1不同的是将步骤（1）中添加的TEOS替换为0.5g醋酸铜，其他均相同。本实施例制备的三维多孔氧化铜材料如图3所示。
实施例15
本实施例的三维多孔材料的制备方法与实施例1不同的是将步骤（1）中添加的TEOS替换为0.5mL四氯化钛，其他均相同。本实施例制备的三维多孔氧化钛材料如图4所示。
实施例16
本实施例的三维多孔材料的制备方法与实施例1不同的是将步骤（1）中添加的TEOS替换为0.5g醋酸镍，其他均相同。本实施例制备的三维多孔氧化镍材料如图5所示。
实施例17
本实施例的三维多孔材料的制备方法与实施例1不同的是将步骤（1）中添加的TEOS替换为0.5g硝酸锌，其他均相同。本实施例制备的三维多孔氧化锌材料如图6所示。
实施例18
本实施例的三维多孔材料的制备方法与实施例1不同的是将步骤（1）添加的TEOS替换为0.5g醋酸铜，将步骤（4）中的空气气氛改为惰性气氛，其他均相同。本实施例制备的三维多孔碳复合材料如图7所示。

Claims (6)

1.一种三维多孔材料的制备方法，其特征在于，包括以下步骤：
（1）将前驱体、PAN、PVP和DMF混合均匀，得混合液A；所述前驱体为硅源、铜源、钛源、镍源、锌源中的一种或几种的组合；
（2）将混合液A均匀填充到模具中，然后将模具浸入到碱性溶液中，保持0.5h，得多孔薄膜，然后煅烧得三维多孔材料。
2.根据权利要求1所述三维多孔材料的制备方法，其特征在于，步骤（1）所述PAN和PVP在混合液A中的总质量分数不低于20%。
3.根据权利要求1所述三维多孔材料的制备方法，其特征在于，步骤（1）所述前驱体在混合液A中的质量分数不低于3%。
4.根据权利要求1所述三维多孔材料的制备方法，其特征在于，步骤（2）所述煅烧为在有氧气氛下，将多孔薄膜在500~700℃温度下保温1~4h。
5.根据权利要求1所述三维多孔材料的制备方法，其特征在于，步骤（2）所述煅烧为在惰性气氛下，将多孔薄膜在500~700℃温度下保温1~4h。
6.根据权利要求4或5所述三维多孔材料的制备方法，其特征在于，所述煅烧的升温速率为1~5℃/min。
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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20140046117A (ko) * 2012-10-10 2014-04-18 한남대학교 산학협력단 금속착물형 탄소기공막 공기정화용 필터 및 그의 제조방법
CN105655153A (zh) * 2016-01-06 2016-06-08 东北师范大学 一种自支撑电容器电极材料的制备方法
CN105958045A (zh) * 2016-06-07 2016-09-21 浙江大学 一种用于锂硫电池的正极材料及其制备方法
CN106324059A (zh) * 2016-08-24 2017-01-11 东北师范大学 一种无酶葡萄糖传感器电极材料的制备方法
CN106345314A (zh) * 2016-09-23 2017-01-25 江苏大学 一种多孔氧化铁‑氧化钛‑活性炭复合纤维膜及制备方法
CN106532104A (zh) * 2015-09-09 2017-03-22 中国科学院大连化学物理研究所 一种锂硫电池用凝胶电解质多孔电极及其制备和应用
CN108114531A (zh) * 2017-12-12 2018-06-05 东南大学 一种多孔纳米光纤异质结构光催化滤网的制备方法
CN108314008A (zh) * 2018-02-09 2018-07-24 北京化工大学 一种柔性可压缩3d全碳纳米纤维气凝胶及其制备方法
CN108385209A (zh) * 2018-03-02 2018-08-10 河南工程学院 多孔纳米碳纤维的制备方法
CN108808008A (zh) * 2018-07-06 2018-11-13 天津大学 一种三维混合离子电子导体集流体及其制备方法和应用

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20140046117A (ko) * 2012-10-10 2014-04-18 한남대학교 산학협력단 금속착물형 탄소기공막 공기정화용 필터 및 그의 제조방법
CN106532104A (zh) * 2015-09-09 2017-03-22 中国科学院大连化学物理研究所 一种锂硫电池用凝胶电解质多孔电极及其制备和应用
CN105655153A (zh) * 2016-01-06 2016-06-08 东北师范大学 一种自支撑电容器电极材料的制备方法
CN105958045A (zh) * 2016-06-07 2016-09-21 浙江大学 一种用于锂硫电池的正极材料及其制备方法
CN106324059A (zh) * 2016-08-24 2017-01-11 东北师范大学 一种无酶葡萄糖传感器电极材料的制备方法
CN106345314A (zh) * 2016-09-23 2017-01-25 江苏大学 一种多孔氧化铁‑氧化钛‑活性炭复合纤维膜及制备方法
CN108114531A (zh) * 2017-12-12 2018-06-05 东南大学 一种多孔纳米光纤异质结构光催化滤网的制备方法
CN108314008A (zh) * 2018-02-09 2018-07-24 北京化工大学 一种柔性可压缩3d全碳纳米纤维气凝胶及其制备方法
CN108385209A (zh) * 2018-03-02 2018-08-10 河南工程学院 多孔纳米碳纤维的制备方法
CN108808008A (zh) * 2018-07-06 2018-11-13 天津大学 一种三维混合离子电子导体集流体及其制备方法和应用

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