CN108385367A - 一种地毯用永久抗菌绒毛面层的制备方法 - Google Patents
一种地毯用永久抗菌绒毛面层的制备方法 Download PDFInfo
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Abstract
一种地毯用永久抗菌绒毛面层的制备方法，属于地毯制备技术。本发明首先将绒毛面层依次用有机溶剂和去离子水超声清洗，再利用原子层沉积技术将清洁后的绒毛面层表面沉积一定厚度的功能纳米ZnO薄膜。由于功能纳米薄膜是通过化学键键合于绒毛面层表面，使其具有良好的化学稳定性，无二次污染，无刺激性，安全无毒，可实现长效广谱抗菌的效果。而且处理后的地毯绒毛面层一定程度上不改变材质的本征特性，如材质的柔软性，光泽及舒适透气性等，具有广阔的应用前景。
Description
技术领域：
本发明涉及一种地毯用永久抗菌绒毛面层的制备方法，属于地毯制备技术。
背景技术
地毯是以羊毛、棉、麻或化学合成纤维，经过手工或机制而成的铺地材料，作为一种居家生活的软装饰品，已经进入生活环境的方方面面，而具有多功能性地毯已经越来越深受人们喜爱，尤其是在抗菌等有优异效果的地毯受到了极大的关注。目前，具有抗菌效应的地毯主要采用后加工整理型，一般都是对地毯纤维材料表面进行改性处理。中国专利公开号CN 202878845U，公开日为2013年4月17日，名称为“一种抗菌复合面料”，所述的抗菌复合面料由PU皮革层、竹炭纤维层和布料层组合而成，其中，竹炭纤维层内填充纳米银微粒，制备的面料具有较好抗菌效果，柔软度和抗拉强度较为优异，但该面料接触油污后，其自清洁效果的能力较差，从而也会影响抗菌能力。中国专利公开号CN 204869854U，公开日是2015年12月16日，名称为“防污耐腐蚀型抗菌复合面料”，该方法采用羊毛层、竹炭纤维层、抗菌层、耐腐蚀层、防污层进行合成，制备的面料层能够保证面料抗菌效果的同时，具备防污、耐腐蚀能力，但制备各功能面层均需要进行改性处理，工艺较为复杂，成本高、生茶效率低。中国专利公开号CN 204049151U，公开日是2014年12月31日，名称为“抗菌地毯”，主要通过在织物地毯表面依次涂覆二氧化硅抗氧化层和光触媒层，使地毯在可见光作用下能够达到抗菌效果，有效净化室内空气，同时具有自清洁的能力，但涂覆在地毯织物表面的功能层容易出现剥离和脱落，从而降低抗菌及自清洁能力。
发明内容
针对上述问题，本发明的目的在于提供一种地毯用永久抗菌绒毛面层的制备方法。
为了实现上述目的，本发明的技术解决方案为，一种地毯用永久抗菌绒毛面层的制备方法，所述方法按以下步骤进行：
步骤A 绒毛面层的清洁化处理
按浴比为1:50-100将绒毛面层置于有机溶剂中超声清洗30-60min，然后在45-80℃条件下干燥2-4h；再将干燥后的绒毛面层按浴比为1:50-100在去离子水中超声清洗30-60min，然后在80-100℃条件下干燥6-10h；
步骤B 绒毛面层的抗菌整理
ZnO薄膜的原子层沉积：
设定的原子层沉积参数为：
反应温度： 60-300℃；
反应源：采用纯度大于97% 的Zn(CH3)2或Zn(C2H5)2或Zn(CH3COO)2或为第一前躯体，H2O或二元醇为第二前驱体，其中，第一前躯体和第二前躯体的源温均为室温；
载气：10-150sccm的高纯氮气，高纯氮气的纯度为99.999%；
将经步骤A得到的绒毛面层放入原子层沉积设备的反应腔，用高纯氮气吹扫3-10min，然后将第一前躯体以脉冲形式送入反应腔体，脉冲时间为0.1-0.4s，暴露时间为15-38s,再用高纯氮气吹扫，吹扫时间为30-50s；再将第二前驱体以脉冲形式送入反应腔体，脉冲时间为1-5s，暴露时间为20-60s，再用高纯氮气吹扫，吹扫时间为20-60s，完成了一次沉积循环。
所用有机溶剂为乙醇或丙醇或乙醚或丙酮或氯仿中的一种。
所述的绒毛面层材质为蚕丝材质、绵羊毛材质、纯棉材质、椰纤材质、竹纤材质、麻纤材质、锦纶材质、涤纶材质、丙纶材质、腈纶材质、橡胶植绒材质、维纶材质、氨纶材质、粘胶材质中的一种。
通过对 ZnO薄膜的原子层沉积过程的多次重复，可以精准控制ZnO薄膜的厚度。
所述的 ZnO薄膜每一个沉积循环生长厚度为0.08-0.12nm。
由于采用以上技术方案，本发明提供的一种地毯用永久抗菌绒毛面层的制备方法的有益效果是:
(1) 本发明制备的锌基功能纳米薄膜具有高的催化活性，良好的化学稳定性和热稳定性，无二次污染，无刺激性，安全无毒，可实现长效广谱抗菌的效果。
(2) 本发明适用材质种类较多，且沉积的锌基功能纳米薄膜在一定程度上不改变材质的本征特性，如材质的柔软性，光泽及舒适透气性等。
(3) 本发明采用的原子层沉积技术，制备工艺简单、操作方便、生产效率高、成本和能耗低，制备的锌基纳米薄膜是通过化学键键合在材质表面，不易洗脱，耐久性好，可有效避免功能纳米薄膜出现剥离或脱落，且分布均匀、薄膜厚度可控，具有极大地应用前景。
具体实施方式
下面结合具体实施例，对本发明作进一步详细描述。
一种地毯用永久抗菌绒毛面层的制备方法，所述制备方法按以下步骤进行：
a 绒毛面层的清洁化处理
将绒毛面层按浴比为1:50-100置于有机溶剂中超声清洗30-60min，然后在45-80℃条件下干燥2-4h；再将干燥后的绒毛面层按浴比为1:50-100在去离子水中超声清洗30-60min，然后在80-100℃条件下干燥6-10h，所用有机溶剂为乙醇或丙醇或乙醚或丙酮或氯仿中的一种，采用的绒毛面层材质为蚕丝材质、绵羊毛材质、纯棉材质、椰纤材质、竹纤材质、麻纤材质、锦纶材质、涤纶材质、丙纶材质、腈纶材质、橡胶植绒材质、维纶材质、氨纶材质、粘胶材质中的一种。
b. 绒毛面层的抗菌整理
将清洁干燥后的绒毛面层放入温度为60-300℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫3-10min，流量为10-150sccm，然后将第一前躯体以脉冲形式送入反应腔体，脉冲时间为0.1-0.4s，暴露时间为15-38s, 再用纯度为99.999%的氮气吹扫，吹扫时间为30-50s，再将第二前驱体以脉冲形式送入反应腔体内，脉冲时间为1-5s，暴露时间为20-60s，再用纯度为99.999%的氮气吹扫，吹扫时间为20-60s，完成了一次沉积循环，ZnO薄膜的生长厚度为0.08-0.12nm，其中，第一前躯体为室温下纯度大于97% 的Zn(CH3)2或Zn(C2H5)2或Zn(CH3COO)2，第二前驱体为室温下的H2O或二元醇。
通过在绒毛面层表面沉积功能纳米ZnO薄膜，使其具有较好的广谱抗菌效果，且功能薄膜主要采用化学键键合的方式形成于绒毛面层表面，不易洗脱，耐久性好，可有效避免功能纳米薄膜出现剥离或脱落，使地毯具有持久的抗菌能力，所制备的薄膜厚度可控、分布均匀，化学稳定性和热稳定性好，对地毯无二次污染，无刺激性，安全无毒，具有较好的应用前景。
实施例1
将蚕丝材质绒毛面层按浴比为1:50置于乙醇中超声清洗30min，然后在45℃条件下干燥2h，将干燥后的蚕丝材质绒毛面层按浴比为1:50在去离子水中超声清洗30min后，放置于80℃条件下干燥6h，将清洁干燥后的蚕丝材质绒毛面层放入温度为60℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫3min，流量为10sccm，然后将处于室温下纯度大于97%的Zn(CH3)2以脉冲形式送入反应腔体内，脉冲时间为0.1s，暴露时间为15s, 再用纯度为99.999%的氮气吹扫，吹扫时间为30s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为1s，暴露时间为20s，再用纯度为99.999%的氮气吹扫，吹扫时间为20s，完成一次沉积循环。按照上述方法重复沉积1000循环，得到功能ZnO薄膜的厚度为90nm的具有永久抗菌效应的地毯绒毛面层。
实施例2
将绵羊毛材质绒毛面层按浴比为1:70置于丙醇中超声清洗60min，然后在80℃条件下干燥4h，将干燥后的绵羊毛材质绒毛面层按浴比为1:100在去离子水中超声清洗60min后，放置于100℃条件下干燥8h，将清洁干燥后的绵羊毛材质绒毛面层放入温度为100℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫5min，流量为30sccm，然后将处于室温下纯度大于97% 的Zn(C2H5)2以脉冲形式送入反应腔体内，脉冲时间为0.4s，暴露时间为20s,再用纯度为99.999%的氮气吹扫，吹扫时间为35s，再将室温条件下的二元醇以脉冲形式送入反应腔体内，脉冲时间为3s，暴露时间为30s，再用纯度为99.999%的氮气吹扫，吹扫时间为30s，完成一次沉积循环。按照上述方法重复沉积2000循环，得到功能ZnO薄膜的厚度为185nm的具有永久抗菌效应的地毯绒毛面层。
实施例3
将纯棉材质绒毛面层按浴比为1:80置于乙醚中超声清洗50min，然后在60℃条件下干燥3h，将干燥后的纯棉材质绒毛面层按浴比为1:80在去离子水中超声清洗60min后，放置于100℃条件下干燥8h，将清洁干燥后的纯棉材质绒毛面层放入温度为120℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫10min，流量为60sccm，然后将处于室温下纯度大于97% 的Zn(CH3COO)2以脉冲形式送入反应腔体内，脉冲时间为0.2s，暴露时间为25s, 再用纯度为99.999%的氮气吹扫，吹扫时间为40s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为5s，暴露时间为50s，再用纯度为99.999%的氮气吹扫，吹扫时间为40s，完成一次沉积循环。按照上述方法重复沉积3000循环，得到功能ZnO薄膜的厚度为273nm的具有永久抗菌效应的地毯绒毛面层。
实施例4
将椰纤材质绒毛面层按浴比为1:100置于乙醚中超声清洗45min，然后在70℃条件下干燥3h，将干燥后的椰纤材质绒毛面层按浴比为1:75在去离子水中超声清洗45min后，放置于90℃条件下干燥10h，将清洁干燥后的椰纤材质绒毛面层放入温度为150℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫6min，流量为80sccm，然后将处于室温下纯度大于97% 的Zn(CH3COO)2以脉冲形式送入反应腔体内，脉冲时间为0.4s，暴露时间为30s, 再用纯度为99.999%的氮气吹扫，吹扫时间为45s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为3s，暴露时间为60s，再用纯度为99.999%的氮气吹扫，吹扫时间为50s，完成一次沉积循环；按照上述方法重复沉积4000循环，得到功能ZnO薄膜的厚度为364nm的具有永久抗菌效应的地毯绒毛面层。
实施例5
将竹纤材质绒毛面层按浴比为1:65置于乙醚中超声清洗40min，然后在70℃条件下干燥2.5h，将干燥后的竹纤材质绒毛面层按浴比为1:85在去离子水中超声清洗55min后，放置于95℃条件下干燥7h，将清洁干燥后的竹纤材质绒毛面层放入温度为180℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫7min，流量为100sccm，然后将处于室温下纯度大于97% 的Zn(C2H5)2以脉冲形式送入反应腔体内，脉冲时间为0.1s，暴露时间为35s, 再用纯度为99.999%的氮气吹扫，吹扫时间为50s，再将室温条件下的二元醇以脉冲形式送入反应腔体内，脉冲时间为5s，暴露时间为45s，再用纯度为99.999%的氮气吹扫，吹扫时间为60s，完成一次沉积循环。按照上述方法重复沉积5000循环，得到功能ZnO薄膜的厚度为456nm的具有永久抗菌效应的地毯绒毛面层。
实施例6
将麻纤材质绒毛面层按浴比为1:60置于丙酮中超声清洗40min，然后在70℃条件下干燥3h，将干燥后的麻纤材质绒毛面层按浴比为1:65在去离子水中超声清洗45min后，放置于80℃条件下干燥8h，将清洁干燥后的麻纤材质绒毛面层放入温度为200℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫4min，流量为120sccm，然后将处于室温下纯度大于97% 的Zn(CH3)2以脉冲形式送入反应腔体内，脉冲时间为0.15s，暴露时间为38s, 再用纯度为99.999%的氮气吹扫，吹扫时间为42s，再将室温条件下的二元醇以脉冲形式送入反应腔体内，脉冲时间为3s，暴露时间为40s，再用纯度为99.999%的氮气吹扫，吹扫时间为45s，完成一次沉积循环。按照上述方法重复沉积6000循环，得到功能ZnO薄膜的厚度为562nm的具有永久抗菌效应的地毯绒毛面层。
实施例7
将锦纶材质绒毛面层按浴比为1:60置于氯仿中超声清洗35min，然后在60℃条件下干燥4h，将干燥后的锦纶材质绒毛面层按浴比为1:95在去离子水中超声清洗45min后，放置于85℃条件下干燥7h，将清洁干燥后的锦纶材质绒毛面层放入温度为240℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫8min，流量为150sccm，然后将处于室温下纯度大于97% 的Zn(CH3)2以脉冲形式送入反应腔体内，脉冲时间为0.25s，暴露时间为32s, 再用纯度为99.999%的氮气吹扫，吹扫时间为48s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为3s，暴露时间为48s，再用纯度为99.999%的氮气吹扫，吹扫时间为55s，完成一次沉积循环。按照上述方法重复沉积7000循环，得到功能ZnO薄膜的厚度为658nm的具有永久抗菌效应的地毯绒毛面层。
实施例8
将涤纶材质绒毛面层按浴比为1:95置于氯仿中超声清洗38min，然后在65℃条件下干燥2h，将干燥后的涤纶材质绒毛面层按浴比为1:90在去离子水中超声清洗48min后，放置于100℃条件下干燥6h，将清洁干燥后的涤纶材质绒毛面层放入温度为270℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫6min，流量为110sccm，然后将处于室温下纯度大于97% 的Zn(CH3COO)2以脉冲形式送入反应腔体内，脉冲时间为0.28s，暴露时间为26s, 再用纯度为99.999%的氮气吹扫，吹扫时间为33s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为3.5s，暴露时间为38s，再用纯度为99.999%的氮气吹扫，吹扫时间为52s，完成一次沉积循环。按照上述方法重复沉积8000循环，得到功能ZnO薄膜的厚度为752nm的具有永久抗菌效应的地毯绒毛面层。
实施例9
将丙纶材质绒毛面层按浴比为1:55置于氯仿中超声清洗40min，然后在75℃条件下干燥2.5h，将干燥后的丙纶材质绒毛面层按浴比为1:60在去离子水中超声清洗56min后，放置于75℃条件下干燥7h，将清洁干燥后的丙纶材质绒毛面层放入温度为300℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫7min，流量为105sccm，然后将处于室温下纯度大于97% 的Zn(CH3COO)2以脉冲形式送入反应腔体内，脉冲时间为0.32s，暴露时间为28s, 再用纯度为99.999%的氮气吹扫，吹扫时间为38s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为4.2s，暴露时间为40s，再用纯度为99.999%的氮气吹扫，吹扫时间为52s，完成一次沉积循环。按照上述方法重复沉积9000循环，得到功能ZnO薄膜的厚度为856nm的具有永久抗菌效应的地毯绒毛面层。
实施例10
将腈纶材质绒毛面层按浴比为1:75置于丙醇中超声清洗40min，然后在65℃条件下干燥3h，将干燥后的腈纶材质绒毛面层按浴比为1:90在去离子水中超声清洗60min后，放置于75℃条件下干燥8h，将清洁干燥后的腈纶材质绒毛面层放入温度为280℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫10min，流量为95sccm，然后将处于室温下纯度大于97% 的Zn(CH3)2以脉冲形式送入反应腔体内，脉冲时间为0.4 s，暴露时间为22s, 再用纯度为99.999%的氮气吹扫，吹扫时间为35s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为4.5s，暴露时间为28s，再用纯度为99.999%的氮气吹扫，吹扫时间为35s，完成一次沉积循环。按照上述方法重复沉积10000循环，得到功能ZnO薄膜的厚度为961nm的具有永久抗菌效应的地毯绒毛面层。
实施例11
将橡胶植绒材质绒毛面层按浴比为1:95置于乙醚中超声清洗38min，然后在75℃条件下干燥2.8h，将干燥后的橡胶植绒材质绒毛面层按浴比为1:90在去离子水中超声清洗60min后，放置于75℃条件下干燥8h，将清洁干燥后的橡胶植绒材质绒毛面层放入温度为260℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫5min，流量为85sccm，然后将处于室温下纯度大于97% 的Zn(CH3)2以脉冲形式送入反应腔体内，脉冲时间为0.25 s，暴露时间为20s, 再用纯度为99.999%的氮气吹扫，吹扫时间为38s，再将室温条件下的二元醇以脉冲形式送入反应腔体内，脉冲时间为2.5s，暴露时间为30s，再用纯度为99.999%的氮气吹扫，吹扫时间为45s，完成一次沉积循环。按照上述方法重复沉积11000循环，得到功能ZnO薄膜的厚度为1100nm的具有永久抗菌效应的地毯绒毛面层。
实施例12
将维纶材质材质绒毛面层按浴比为1:70置于乙醇中超声清洗50min，然后在70℃条件下干燥3h，将干燥后的维纶材质绒毛面层按浴比为1:95在去离子水中超声清洗55min后，放置于85℃条件下干燥6h，将清洁干燥后的维纶材质绒毛面层放入温度为250℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫4min，流量为80sccm，然后将处于室温下纯度大于97% 的Zn(C2H5)2以脉冲形式送入反应腔体内，脉冲时间为0.32 s，暴露时间为25s, 再用纯度为99.999%的氮气吹扫，吹扫时间为40s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为2.6s，暴露时间为35s，再用纯度为99.999%的氮气吹扫，吹扫时间为48s，完成一次沉积循环。按照上述方法重复沉积12000循环，得到功能ZnO薄膜的厚度为1210nm的具有永久抗菌效应的地毯绒毛面层。
实施例13
将氨纶材质绒毛面层按浴比为1:50置于丙酮中超声清洗60min，然后在50℃条件下干燥2h，将干燥后的氨纶材质绒毛面层按浴比为1:65在去离子水中超声清洗50min后，放置于85℃条件下干燥7h，将清洁干燥后的氨纶材质绒毛面层放入温度为250℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫5min，流量为60sccm，然后将处于室温下纯度大于97% 的Zn(C2H5)2以脉冲形式送入反应腔体内，脉冲时间为0.2 s，暴露时间为25s, 再用纯度为99.999%的氮气吹扫，吹扫时间为46s，再将室温条件下的二元醇以脉冲形式送入反应腔体内，脉冲时间为2.6s，暴露时间为35s，再用纯度为99.999%的氮气吹扫，吹扫时间为52s，完成一次沉积循环。按照上述方法重复沉积13000循环，得到功能ZnO薄膜的厚度为1330nm的具有永久抗菌效应的地毯绒毛面层。
实施例14
将粘胶材质绒毛面层按浴比为1:80置于氯仿中超声清洗60min，然后在70℃条件下干燥2h，将干燥后的粘胶材质绒毛面层按浴比为1:65在去离子水中超声清洗50min后，放置于85℃条件下干燥7h，将清洁干燥后的粘胶材质绒毛面层放入温度为250℃原子层沉积设备的反应腔，用纯度为99.999%的氮气吹扫5min，流量为50sccm，然后将处于室温下纯度大于97% 的Zn(CH3COO)2以脉冲形式送入反应腔体内，脉冲时间为0.2 s，暴露时间为25s, 再用纯度为99.999%的氮气吹扫，吹扫时间为40s，再将室温条件下的H2O以脉冲形式送入反应腔体内，脉冲时间为2.6s，暴露时间为35s，再用纯度为99.999%的氮气吹扫，吹扫时间为42s，完成一次沉积循环。按照上述方法重复沉积14000循环，得到功能ZnO薄膜的厚度为1480nm的具有永久抗菌效应的地毯绒毛面层。
Claims (5)
1. 一种地毯用永久抗菌绒毛面层的制备方法，其特征在于：所述制备方法按以下步骤进行：
步骤A 绒毛面层的清洁化处理
按浴比为1:50-100将绒毛面层置于有机溶剂中超声清洗30-60min，然后在45-80℃条件下干燥2-4h；再将干燥后的绒毛面层按浴比为1:50-100在去离子水中超声清洗30-60min，然后在80-100℃条件下干燥6-10h；
步骤B 绒毛面层的抗菌整理
ZnO薄膜的原子层沉积：
设定的原子层沉积参数为：
反应温度： 60-300℃；
反应源：采用纯度大于97% 的Zn(CH3)2或Zn(C2H5)2或Zn(CH3COO)2或为第一前躯体，H2O或二元醇为第二前驱体，其中，第一前躯体和第二前躯体的源温均为室温；
载气：10-150sccm的高纯氮气，高纯氮气的纯度为99.999%；
将经步骤A得到的绒毛面层放入原子层沉积设备的反应腔，用高纯氮气吹扫3-10min，然后将第一前躯体以脉冲形式送入反应腔体，脉冲时间为0.1-0.4s，暴露时间为15-38s,再用高纯氮气吹扫，吹扫时间为30-50s；再将第二前驱体以脉冲形式送入反应腔体，脉冲时间为1-5s，暴露时间为20-60s，再用高纯氮气吹扫，吹扫时间为20-60s，完成了一次沉积循环。
2.如权利要求1所述的一种地毯用永久抗菌绒毛面层的制备方法，其特征在于：所用有机溶剂为乙醇或丙醇或乙醚或丙酮或氯仿中的一种。
3.如权利要求1所述的一种地毯用永久抗菌绒毛面层的制备方法，其特征在于：所述的绒毛面层材质为蚕丝材质、绵羊毛材质、纯棉材质、椰纤材质、竹纤材质、麻纤材质、锦纶材质、涤纶材质、丙纶材质、腈纶材质、橡胶植绒材质、维纶材质、氨纶材质、粘胶材质中的一种。
4.如权利要求1所述的一种地毯用永久抗菌绒毛面层的制备方法，其特征在于：通过对ZnO薄膜的原子层沉积过程的多次重复，可以精准控制ZnO薄膜的厚度。
5.如权利要求1所述的一种地毯用永久抗菌绒毛面层的制备方法，其特征在于：所述的ZnO薄膜每一个沉积循环生长厚度为0.08-0.12nm。
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