CN109576984A - 一种耐久型ZnO纳米线阵列材料的制备方法 - Google Patents
一种耐久型ZnO纳米线阵列材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种耐久型ZnO纳米线阵列材料的制备方法，包括将基材加入到MAPS和有机溶剂组成的混合溶液中进行γ射线辐照，使得MAPS通过共价键接枝到基材上形成接枝样品；将强碱和锌盐分别溶解在乙醇溶液中后混合得到ZnO种子溶胶，将接枝样品浸入ZnO种子溶胶中，使得接枝样品的表面通过化学键锚固一层ZnO种子层，得到负载ZnO样品；将锌盐、六次甲基四胺、负载ZnO样品加入水热反应釜中，使得负载ZnO样品的表面原位生长ZnO纳米线阵列，得到耐久型ZnO纳米线阵列材料。本发明采用MAPS作为桥连剂，将ZnO种子层通过化学键锚固在基材的表面，从而赋予一维ZnO纳米线阵列超高的耐久性。
Description
技术领域
本发明涉及高分子材料表面改性，更具体地涉及一种耐久型ZnO纳米线阵列材料的制备方法。
背景技术
由于一维纳米材料出色的光学性能、磁学性能、力学性能、电学性能、光电性能等性质，使其在光催化、电化学、光致发光及各种传感器等领域展示出极大的发展潜力。目前，合成出来的一维氧化锌纳米材料包括纳米棒、纳米线、纳米带、纳米环、纳米阵列等一维结构。一般地，随着尺寸的减小，一维ZnO纳米结构会表现出比宏观材料更好的发光性能、导电性能及光电性能，而被应用于发光二极管、紫外探测器以及荧光标记生物材料等。
近年来，将一维ZnO纳米线阵列在韧性基材表面(例如：织物、塑料、纸)原位生长，来制备柔性、质轻的功能复合材料，如：紫外吸收、自清洁、超疏水、抗菌织物、铀吸附材料等。例如，Wang等在棉织物表面原位生长氧化锌纳米线阵列来吸附铀酰离子(L.Z.LeiZhang,Liang Zhang,Tianhao Wu,Xiaoyan Jing,Rumin Li,Jingyuan Liu,Qi Liu andJun Wang.In situ growth of ZnO nanorod arrays on cotton cloth for the removalof uranium(VI))。尽管在柔性基材表面原位生长一维ZnO纳米线阵列能够赋予材料一定的新功能性，但仍然存在一些难以解决的问题。首先，在ZnO纳米线阵列与基材之间没有化学键，这导致ZnO在材料表面的耐久性较差，在外力的作用下纳米线易于从基材表面剥离，从而使材料失去功能性。其次，ZnO具有较高的光催化性能，光催化过程中产生的空穴会降解负载ZnO纳米线的有机载体，从而导致功能材料力学性能丧失。
发明内容
为了解决上述现有技术存在的一维ZnO纳米线阵列易于从基材表面剥离的问题，本发明旨在提供一种耐久型ZnO纳米线阵列材料的制备方法。
本发明所述的耐久型ZnO纳米线阵列材料的制备方法，包括步骤：S1，将基材加入到3-甲基丙烯酰氧基丙基三甲氧基硅烷(MAPS)和有机溶剂组成的混合溶液中进行γ射线辐照，使得3-甲基丙烯酰氧基丙基三甲氧基硅烷(MAPS)通过共价键接枝到基材上形成接枝样品(PMAPS)；S2，将强碱和锌盐分别溶解在乙醇溶液中后混合得到ZnO种子溶胶，将接枝样品浸入ZnO种子溶胶中，使得接枝样品(PMAPS)的表面通过化学键锚固一层ZnO种子层，得到负载ZnO样品；S3，将锌盐、六次甲基四胺、负载ZnO样品加入水热反应釜中，使得负载ZnO样品的表面原位生长ZnO纳米线阵列，得到耐久型ZnO纳米线阵列材料。
所述步骤S1包括：将100份基材(SUB)加入到由1043-2086份3-甲基丙烯酰氧基丙基三甲氧基硅烷(MAPS)和6304-7092份有机溶剂组成的混合溶液中，在室温下通惰性气体10-20min后，放置于钴源下辐照，吸收剂量为10-50kGy。
所述有机溶剂为甲醇、乙醇或丙酮。
所述惰性气体为氮气或氩气。
所述基材为聚乙烯纤维、聚丙烯纤维、尼龙纤维、棉布、聚偏氟乙烯纤维、或芳砜基纤维。在优选的实施例中，所述基材为聚对苯二甲酸乙二酯(PET)织物或超高分子量聚乙烯(UHMWPE)纤维。应该理解，除了上面列举出的基材，还可以是其他能够通过辐射接枝聚合方法在基材表面引入PMAPS分子链的聚合物材料。
所述步骤S1还包括：所述基材在60-65℃下，于低沸点溶剂中抽提12-24h以洗掉基材表面的油脂和杂质，在50-60℃下烘干0.5-1h后加入到混合溶液中。
所述低沸点溶剂为甲醇、乙醇或丙酮。
所述步骤S1还包括：接枝样品在清洗溶剂中超声清洗0.5-1h后，在40-50℃下烘干2-3h。
所述清洗溶剂为甲醇、乙醇、丙酮或其混合物。
所述步骤S2包括：14.4-20份NaOH和88-100份锌盐分别溶解在79-95份和158-200份的乙醇溶液中，将上述的两种溶液混合，并在50-60℃下搅拌3-5h，得到ZnO种子溶胶；将100份接枝样品浸入ZnO种子溶胶中5-15分钟，取出后在120-160℃下加热10-20min，得到负载ZnO样品。
所述锌盐为醋酸锌或六水硝酸锌。在优选的实施例中，所述锌盐为Zn(CH3COO)2·2H2O。
所述步骤S3包括：将458-750份的锌盐和350-450份六次甲基四胺溶解在8000-10000份去离子水中的溶液加入水热反应釜中，将100-150份负载ZnO样品加入水热反应釜中，密闭水热反应釜，在90-105℃下反应4-7h，得到耐久型ZnO纳米线阵列材料。
所述锌盐为醋酸锌或六水硝酸锌。在优选的实施例中，所述锌盐为Zn(CH3COO)2·2H2O。
所述步骤S3还包括：耐久型ZnO纳米线阵列材料在清洗溶剂中超声清洗1-1.5h后，在40-60℃下烘干2-4h。
所述清洗溶剂为甲醇、乙醇、丙酮或其混合物。
本发明采用共辐照接枝聚合的方法，将MAPS通过共价键引入到基材表面，然后采用溶胶-凝胶法在PMAPS表面锚固一层ZnO种子层，最后在水热釜中定向生长ZnO纳米线阵列。具体地，本发明采用MAPS作为桥连剂，一方面，MAPS的甲基丙烯酰氧基在γ射线辐照下，在柔性的基材的表面进行接枝聚合反应，从而把PMAPS接枝链通过共价键锚固到基材的表面；另一方面，硅甲基易于与锌盐(ZnO的前驱体)通过缩合反应生成Si-O-Zn化学键，将ZnO种子层通过化学键锚固在基材的表面，从而赋予一维ZnO纳米线阵列超高的耐久性。另外，在PMAPS接枝链和种子层之间存在由Si-O-Si及Si-O-Zn组成的界面层，此界面层的Si-O的键能大于Zn-O的键能，能够有效的阻止ZnO纳米线阵列在吸收紫外光的过程中，ZnO受到激发产生的空穴对有机载体的降解作用。特别地，本发明采用共辐照接枝手段在较低的剂量下接枝MAPS，最大程度的减小辐照对基材降解的影响。而且，通过接枝双官能团的硅烷偶联剂MAPS，一方面提高了纳米线阵列与基材之间界面结合力，同时又克服了ZnO纳米线阵列对有机载体的自降解作用。
附图说明
图1是根据本发明的耐久型ZnO纳米线阵列材料的扫描电子显微镜照片；
图2是图1的局部放大图。
具体实施方式
下面结合附图，给出本发明的较佳实施例，并予以详细描述。
实施例1
将100份聚对苯二甲酸乙二酯(PET)织物，在60℃下，于丙酮中抽提12h。所得的样品在50℃下烘干0.5h后备用。将100份经过抽提的PET织物加入到由1043份3-甲基丙烯酰氧基丙基三甲氧基硅烷(MAPS)和7092份丙酮组成的混合溶液中。上述体系在室温下通氮气10min后，放置于钴源辐照，吸收剂量10kGy。接枝样品使用乙醇超声清洗0.5h后，在40℃下烘干2h，得到接枝MAPS的样品，接枝样品记为PET-g-PMAPS。
PET-g-PMAPS表面负载ZnO晶种：14.4份NaOH和88份Zn(CH3COO)2·2H2O分别溶解在79份和158份的乙醇中。将上述的两种溶液混合，并在50℃下搅拌3h，得到ZnO种子溶胶。将100份PET-g-PMAPS基材浸入种子溶胶中5分钟，取出PET-g-PMAPS并在120℃下加热20min。上述过程重复2次。所得样品记为PET-g-PMAPS/C-ZnO。
在PET-g-PMAPS/C-ZnO表面原位生长ZnO纳米线阵列：458份的Zn(CH3COO)2·2H2O和350份六次甲基四胺溶解在8000份去离子水中，充分溶解后，将溶液加入水热反应釜中。将100份PET-g-PMAPS/C-ZnO加入上述水热釜中后，密闭反应釜，并在90℃下反应4h。样品取出，并在去离子水中超声清洗1h，在40℃下烘干2h，所得样品记为PET-g-PMAPS/ZnO。
图1是根据本实施例的样品PET-g-PMAPS/ZnO的扫描电子显微镜照片，图2是图1的局部放大图，显然，根据本实施例的方法可以在表面光滑的PET纤维的表面生长一层均匀的氧化锌纳米线阵列，而且，该氧化锌纳米线阵列均匀地负载到PET纤维的表面。
实施例2
将100份超高分子量聚乙烯(UHMWPE)纤维，在65℃下，于乙醇中抽提24h。所得的样品在60℃下烘干1h后备用。将100份经过抽提的UHMWPE纤维加入到由2086份MAPS和6304份甲醇组成的混合溶液中。上述体系在室温下通氩气20min后，放置于钴源辐照，吸收剂量50kGy。接枝样品使用甲醇超声清洗1h后，在50℃下烘干3h，得到接枝MAPS的样品，接枝样品记为UHMWPE-g-PMAPS。
UHMWPE-g-PMAPS表面负载ZnO晶种：20份NaOH和100份六水硝酸锌分别溶解在95份和200份的乙醇中。将上述的两种溶液混合，并在60℃下搅拌5h，得到ZnO种子溶胶。将100份UHMWPE-g-PMAPS基材浸入种子溶胶中15分钟，取出UHMWPE-g-PMAPS并在160℃下加热10min。上述过程重复4次。所得样品记为UHMWPE-g-PMAPS/C-ZnO。
在UHMWPE-g-PMAPS/C-ZnO表面原位生长ZnO纳米线阵列：750份的六水硝酸锌和450份六次甲基四胺溶解在10000份去离子水中，充分溶解后，将溶液加入水热反应釜中。将150份UHMWPE-g-PMAPS/C-ZnO加入上述水热釜中后，密闭反应釜，并在105℃下反应7h。样品取出，并在溶剂中超声清洗1.5h，在60℃下烘干4h，所得样品记为UHMWPE-g-PMAPS/ZnO。
实施例3
将100份尼龙(Ny)纤维，在60℃下，于甲醇中抽提24h。所得的样品在50℃下烘干1h后备用。将100份样品加入到由1500份MAPS和6500份乙醇组成的混合溶液中。上述体系在室温下通氩气20min后，放置于钴源辐照，吸收剂量30kGy。接枝样品使用乙醇溶液超声清洗0.5h后，在45℃下烘干2h，得到接枝MAPS的样品，接枝样品记为Ny-g-PMAPS。
Ny-g-PMAPS表面负载ZnO晶种：16份NaOH和92份Zn(CH3COO)2·2H2O分别溶解在88份和180份的乙醇中。将上述的两种溶液混合，并在55℃下搅拌4h，得到ZnO种子溶胶。将100份Ny-g-PMAPS基材浸入种子溶胶中10分钟，取出Ny-g-PMAPS并在130℃下加热15min。上述过程重复3次。所得样品记为Ny-g-PMAPS/C-ZnO。
在Ny-g-PMAPS/C-ZnO表面原位生长ZnO纳米线阵列：550份的Zn(CH3COO)2·2H2O和400份六次甲基四胺溶解在10000份去离子水中，充分溶解后，将溶液加入水热反应釜中。将120份Ny-g-PMAPS/C-ZnO加入上述水热釜中后，密闭反应釜，并在100℃下反应6h。样品取出，并在乙醇中超声清洗1h，在50℃下烘干3h，所得样品记为Ny-g-PMAPS/ZnO。
实施例4
将100份棉布(Cot)，在60℃下，于甲醇中抽提24h。所得的样品在60℃下烘干1h后备用。将100份经过抽提的棉布加入到由1500份MAPS和6600份丙酮组成的混合溶液中。上述体系在室温下通氮气15min后，放置于钴源辐照，吸收剂量40kGy。接枝样品使用溶剂超声清洗1h后，在45℃下烘干2h，得到接枝MAPS的样品，接枝样品记为Cot-g-PMAPS。
Cot-g-PMAPS表面负载ZnO晶种：16份NaOH和92份Zn(CH3COO)2·2H2O分别溶解在95份和158份的乙醇中。将上述的两种溶液混合，并在55℃下搅拌5h，得到ZnO种子溶胶。将100份Cot-g-PMAPS基材浸入种子溶胶中5分钟，取出Cot-g-PMAPS并在130℃下加热15min。上述过程重复3次。所得样品记为Cot-g-PMAPS/C-ZnO。
在Cot-g-PMAPS/C-ZnO表面原位生长ZnO纳米线阵列：650份的Zn(CH3COO)2·2H2O和450份六次甲基四胺溶解在10000份去离子水中，充分溶解后，将溶液加入水热反应釜中。将110份Cot-g-PMAPS/C-ZnO加入上述水热釜中后，密闭反应釜，并在100℃下反应6h。样品取出，并在溶剂中超声清洗1h，在40℃下烘干4h，所得样品记为Cot-g-PMAPS/ZnO。
实施例5
将100份芳砜基纤维(ASF)，在65℃下，于丙酮溶液中抽提18h。所得的样品在60℃下烘干1h后备用。将100份经过抽提的芳砜基纤维加入到由2086份MAPS和6304份丙酮组成的混合溶液中。上述体系在室温下通氩气10min后，放置于钴源辐照，吸收剂量50kGy。接枝样品使用乙醇超声清洗1h后，在40℃下烘干2h，得到接枝MAPS的样品，接枝样品记为ASF-g-PMAPS。
ASF-g-PMAPS表面负载ZnO晶种：18份NaOH和100份Zn(CH3COO)2·2H2O分别溶解在90份和160份的乙醇中。将上述的两种溶液混合，并在55℃下搅拌4h，得到ZnO种子溶胶。将100份ASF-g-PMAPS基材浸入种子溶胶中10分钟，取出ASF-g-PMAPS并在150℃下加热10min。上述过程重复4次。所得样品记为ASF-g-PMAPS/C-ZnO。
在ASF-g-PMAPS/C-ZnO表面原位生长ZnO纳米线阵列：750份的Zn(CH3COO)2·2H2O和450份六次甲基四胺溶解在10000份去离子水中，充分溶解后，将溶液加入水热反应釜中。将130份ASF-g-PMAPS/C-ZnO加入上述水热釜中后，密闭反应釜，并在100℃下反应7h。样品取出，并在溶剂中超声清洗1.5h，在50℃下烘干3h，所得样品记为ASF-g-PMAPS/ZnO。
以上所述的，仅为本发明的较佳实施例，并非用以限定本发明的范围，本发明的上述实施例还可以做出各种变化。即凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰，皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。
Claims (8)
1.一种耐久型ZnO纳米线阵列材料的制备方法，其特征在于，该制备方法包括步骤：
S1，将基材加入到3-甲基丙烯酰氧基丙基三甲氧基硅烷和有机溶剂组成的混合溶液中进行γ射线辐照，使得3-甲基丙烯酰氧基丙基三甲氧基硅烷通过共价键接枝到基材上形成接枝样品；
S2，将强碱和锌盐分别溶解在乙醇溶液中后混合得到ZnO种子溶胶，将接枝样品浸入ZnO种子溶胶中，使得接枝样品的表面通过化学键锚固一层ZnO种子层，得到负载ZnO样品；
S3，将锌盐、六次甲基四胺、负载ZnO样品加入水热反应釜中，使得负载ZnO样品的表面原位生长ZnO纳米线阵列，得到耐久型ZnO纳米线阵列材料。
2.根据权利要求1所述的制备方法，其特征在于，所述基材为聚乙烯纤维、聚丙烯纤维、尼龙纤维、棉布、聚偏氟乙烯纤维、或芳砜基纤维。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤S1包括：将100份基材加入到由1043-2086份3-甲基丙烯酰氧基丙基三甲氧基硅烷和6304-7092份有机溶剂组成的混合溶液中，在室温下通惰性气体10-20min后，放置于钴源下辐照，吸收剂量为10-50kGy。
4.根据权利要求3所述的制备方法，其特征在于，所述步骤S1还包括：所述基材在60-65℃下，于低沸点溶剂中抽提12-24h以洗掉基材表面的油脂和杂质，在50-60℃下烘干0.5-1h后加入到混合溶液中。
5.根据权利要求3所述的制备方法，其特征在于，所述步骤S1还包括：接枝样品在清洗溶剂中超声清洗0.5-1h后，在40-50℃下烘干2-3h。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤S2包括：14.4-20份NaOH和88-100份锌盐分别溶解在79-95份和158-200份的乙醇溶液中，将上述的两种溶液混合，并在50-60℃下搅拌3-5h，得到ZnO种子溶胶；将100份接枝样品浸入ZnO种子溶胶中5-15分钟，取出后在120-160℃下加热10-20min，得到负载ZnO样品。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤S3包括：将458-750份的锌盐和350-450份六次甲基四胺溶解在8000-10000份去离子水中的溶液加入水热反应釜中，将100-150份负载ZnO样品加入水热反应釜中，密闭水热反应釜，在90-105℃下反应4-7h，得到耐久型ZnO纳米线阵列材料。
8.根据权利要求7所述的制备方法，其特征在于，所述步骤S3还包括：耐久型ZnO纳米线阵列材料在清洗溶剂中超声清洗1-1.5h后，在40-60℃下烘干2-4h。
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