CN109453413A - 一种含微电池的电活性敷料的制备方法 - Google Patents
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Abstract
一种含微电池的电活性敷料的制备方法,属于医用材料制备技术领域。所述方法为:将高分子纤维敷料基材置于真空干燥箱中干燥,使其含水量低于0.01%;在得到的高分子纤维敷料基材表面覆盖Ag限域模板,然后置于溅射设备真空室,氧气/氩气混合氛围下进行溅射;在得到的材料表面覆盖Zn限域模板,然后置于溅射设备真空室在氩气氛围下进行溅射。本发明的优点是:本发明方法通过结合模板限域和磁控溅射直接在高分子纤维基材表面构筑Ag/Zn点电池阵列微电池,赋予敷料电活性,解决现有电活性敷料需外部电源/电池,柔顺性差,贴合不紧密,电流不稳定,使用不方便等问题,并且制备过程条件温和,易于工业化推广,具有广阔的社会效益和经济价值。
Description
技术领域
本发明属于医用材料制备技术领域,具体涉及一种含微电池的电活性敷料的制备方法。
背景技术
皮肤创面存在内源性生物电场,其中心为负极。损伤发生后,电阻抗屏障消失,跨上皮电势差发生短路,电荷/带电离子在电势差的驱动下发生流动即形成了电流。研究发现,内源性电场对损伤部位细胞的迁移发挥了主导性的调控作用,且增强该电场可显著加速伤口愈合。
目前,在一些公开或授权的发明专利中,已经使用如电刺激仪器/设备(CN200480024325.8、CN201710267904.4)、驻极体(CN201520200450.5、CN201711250783.9、CN201520885139.9)、导电高分子(CN201610259364.0、CN201180034211.1)、压电材料(CN201210385628.9)等增强内源性电场或制备电活性敷料,用于促进创面愈合。但目前在临床创面治疗中大多使用电极和导电基底外接电源进行电刺激,需要外接导线,制造及使用不方便,且所用电流与电压过高或不均,易对病患造成不适感并加重伤口疼痛感。此外,现有电活性敷料无法保证敷料的柔软舒适性,贴合性差、干燥、容易产生二次创伤以及不适感。Ag和Zn组成的电池产生的电场已被证明对人体是安全可靠的,如果将Ag和Zn组成的微电池构筑于高分子纤维敷料表面,有望得到一种具有电刺激治疗作用的含微电池的电活性敷料。
发明内容
本发明的目的是为了解决现有电活性敷料需外接电源、电场分布不均、柔软舒适性及贴合性差、制造及使用不方便等问题,提供一种含微电池的电活性敷料的制备方法。
为实现上述目的,本发明采取的技术方案如下:
一种含微电池的电活性敷料的制备方法,所述方法具体步骤为:
步骤一:将高分子纤维敷料基材置于真空干燥箱中30~105℃下干燥,使其含水量低于0.01%;
步骤二:在步骤一得到的高分子纤维敷料基材表面覆盖Ag限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为Ag靶,真空度为1×10-3~1×10-4Pa,溅射气氛为氧气和氩气的混合气体,氩气流量为15~50sccm,氧气与氩气的通入比例为:1/1~2/1之间,溅射功率为30~100W,溅射时间为15~120min,即得到含有Ag电极圆点阵列的高分子纤维敷料;所述的Ag限域模板上包含直径为1~3mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列;
步骤三:在步骤二得到的含Ag电极圆点阵列的高分子纤维敷料表面覆盖Zn限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为Zn靶,真空度为1×10-3~1×10- 4Pa,溅射气氛为氩气,氩气流量为15~50sccm,溅射功率为50~130W,溅射时间为15~120min,即得到含微电池的电活性敷料;所述的Zn限域模板上包含直径为0.5~1.5mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列。
进一步地,步骤一中,所述的高分子纤维敷料基材为纤维素纤维、再生纤维素纤维、氧化纤维素纤维、氧化再生纤维素纤维、海藻纤维、壳聚糖纤维、蚕丝纤维、丙纶纤维、聚乙烯醇纤维、聚酯纤维等的单一/混纺织物或其非织造物。
进一步地,步骤三中,所述的Ag限域模板上的电极微孔阵列的微孔直径始终为Zn限域模板上的电极微孔阵列的微孔直径的1~2倍。
进一步地,步骤三所得电活性敷料上Ag电极圆点与相邻的Zn电极圆点之间的圆心距为1~3.25mm,也就是说,Ag限域模板上的微孔与Zn限域模板上的微孔错位设置,需保证所得电活性敷料上Ag电极圆点阵列与Zn电极圆点阵列不重合,此处,步骤二和步骤三中,使用的模板上是微孔,做成电活性敷料微孔呈现为一个个圆点。
本发明相对于现有技术的有益效果是:
(1)本发明方法通过结合模板限域和磁控溅射直接在高分子纤维基材表面构筑点电极阵列,所构筑的Ag/Zn电池阵列在接触到血液或者伤口渗出液以后会引发氧化还原反应,产生自主持续性放电,赋予敷料稳定的自放电性能,解决现有电活性敷料需外部电源/电池,使用不方便等问题。
(2)本发明方法制备的含微电池的电活性敷料表面的每个阵列电极都是由纳米尺度颗粒堆积而成,分散均匀,解决现有电活性敷料电流过大及不稳定的问题,更有利于产生均匀的电刺激。
(3)本发明方法制备的含微电池的电活性敷料在基材表面直接构筑微电池阵列不会影响基材的柔顺性,解决了现有电活性敷料电极片多层复合导致的柔顺性差、与创面贴合不紧密的问题,并可以任意剪裁,满足不同面积和类型的伤口/创面使用需求。
(4)本发明方法制备的含微电池的电活性敷料产生的电刺激既能抑菌,又能促进组织细胞分裂、增殖、向创面/伤口中心迁移,从而促进创面愈合。
(5)本发明方法制备过程简单、温和,易于工业化推广,具有广阔的社会效益和经济价值。
附图说明
图1为含微电池的电活性敷料制备过程示意图,其中,A-高分子纤维敷料基材、B-Ag@生物敷料基材、C-Ag/Zn@生物敷料基材、E-Ag限域模板、F-Zn限域模板;
图2为本发明制备的含微电池的电活性敷料的照片。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明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精神和范围,均应涵盖在本发明的保护范围中。
本发明的原理是结合模板限域和磁控溅射技术在高分子纤维敷料基材表面构筑Ag/Zn电极阵列,在与血液或伤口渗出液接触以后引发以下一系列的氧化还原反应,产生持续性放电,增强伤口内源性电场,促进细胞迁移和生长,促进创面愈合。
Ag2O+H2O+2e-→2Ag+2OH-
2AgO+H2O+2e-→Ag2+2OH-
Zn+2OH-→ZnO+H2O+2e-
具体实施方式一:本实施方式记载的是一种含微电池的电活性敷料的制备方法,如图1所示,所述方法具体步骤为:
步骤一:将高分子纤维敷料基材置于真空干燥箱中30~105℃下干燥,使其含水量低于0.01%;
步骤二:在步骤一得到的高分子纤维敷料基材表面覆盖Ag限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为99.99%的Ag靶,真空度为1×10-3~1×10-4Pa,溅射气氛为氧气和氩气的混合气体,氩气流量为15~50sccm,氧气与氩气的通入比例为:1/1~2/1之间,溅射功率为30~100W,溅射时间为15~120min,即得到含有Ag电极圆点阵列的高分子纤维敷料;所述的Ag限域模板上包含直径为1~3mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列;
步骤三:在步骤二得到的含Ag电极微孔阵列的高分子纤维敷料表面覆盖Zn限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为99.99%的Zn靶,真空度为1×10-3~1×10-4Pa,溅射气氛为氩气,氩气流量为15~50sccm,溅射功率为50~130W,溅射时间为15~120min,即得到含微电池的电活性敷料;所述的Zn限域模板上包含直径为0.5~1.5mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列。
具体实施方式二:具体实施方式一所述的一种含微电池的电活性敷料的制备方法,步骤一中,所述的高分子纤维敷料基材为纤维素纤维、再生纤维素纤维、氧化纤维素纤维、氧化再生纤维素纤维、海藻纤维、壳聚糖纤维、蚕丝纤维、丙纶纤维、聚乙烯醇纤维、聚酯纤维等的单一/混纺织物或其非织造物。
具体实施方式三:具体实施方式一所述的一种含微电池的电活性敷料的制备方法,步骤三中,所述的Ag限域模板上的电极微孔阵列的微孔直径始终为Zn限域模板上的电极微孔阵列的微孔直径的1~2倍。
具体实施方式四:具体实施方式三所述的一种含微电池的电活性敷料的制备方法,步骤三所得电活性敷料上Ag电极圆点与相邻的Zn电极圆点之间的圆心距为1~3.25mm,也就是说,Ag限域模板上的微孔与Zn限域模板上的微孔错位设置,需保证所得电活性敷料上Ag电极圆点阵列与Zn电极圆点阵列不重合,此处,步骤二和步骤三中,使用的模板上是微孔,做成电活性敷料微孔呈现为一个个圆点,如图2所示。
实施例1:
步骤一:将纤维素纤维织物置于真空干燥箱中35℃干燥,使其含水量低于0.01%;
步骤二:在步骤一得到的纤维素纤维织物表面覆盖孔径为2mm,圆心距为3mm的Ag限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为99.99%的Ag靶,背景压强为1×10-4Pa,氩气流量为30sccm,氧气与氩气的通入比例为1/1之间,溅射功率为30W,溅射时间为15min;
步骤三:在步骤二得到的纤维素纤维织物表面覆盖孔径为1mm,圆心距为4mm的Zn限域模板,确保Zn限域模板上Zn孔与Ag孔圆心距为2mm,然后置于溅射设备真空室,使用直流靶位,选用靶材为99.99%的Zn靶,背景压强为1×10-4Pa,氩气流量为30sccm,溅射功率为50W,溅射时间为15min,得到含微电池的电活性敷料,所得产品标为A。
实施例2:本实施例与实施例1不同之处在于:步骤一和步骤二中的溅射时间均为30min,所得产品标为B。
实施例3:本实施例与实施例1不同之处在于:步骤二中,所述纤维素纤维织物改为海藻纤维无纺布,所得产品标为C。
对以上实施例得到的产品进行测试:
电活性测试:将敷料样品(1x1cm)放入培养皿,加入人体组织模拟液润湿,使用万用表测量两个相邻电极间的电流密度和电压。通过测量及计算发现每个正负极电极可产生1.5~100μA/cm2的电流和20~300mV/mm的电压,与皮肤内源性电流和电压接近,且不会对人体产生刺激感。
动物伤口愈合实验:以SD大鼠为动物模型测试本发明实施例制备的含微电池的电活性敷料对伤口的促愈作用。用10%(w/v)水合氯醛腹腔注射(0.3mL/100g)将SD大鼠(体重200g左右)麻醉,背部脱毛,俯卧位固定于实验操作台上,背部消毒后于脊柱两侧等距离部位,切割两个伤口(1cm×1cm),贴敷样品A、B、C及脱脂棉纱布,大鼠分笼饲养,不禁食,不禁水。创面大小采用相机拍摄照片记录,并使用Image J医学图像分析软件测算创面愈合率。创面愈合率=(1-St/S0)x100%,其中St为t时刻创面面积、S0为初始创面面积。
表1创面愈合率计算结果
组别 | 3d | 7d | 10d | 14d |
脱脂棉纱布 | 15.98±2.19 | 34.27±3.34 | 78.93±5.36 | 92.25±3.67 |
样品A | 18.76±1.87 | 43.91±2.11 | 82.41±3.04 | 94.08±1.65 |
样品B | 26.57±4.01 | 48.69±3.09 | 88.36±5.39 | 98.03±3.28 |
样品C | 23.76±2.03 | 45.97±6.07 | 83.36±7.01 | 96.01±4.01 |
由表1试验结果可知本发明制备的含微电池的电活性敷料比同期脱脂棉纱布敷料治疗创面的愈合率高,证明含微电池的电活性敷料对伤口愈合的促进作用更加明显。
抗菌性能测试:将脱脂棉纱布和实施例样品剪成直径25mm的圆型试样,在超净工作台紫外照射30min灭菌。在固体LB培养基上滴取100μL浓度为1×108CFU/mL的实验室菌悬液(金黄色葡萄球菌或大肠杆菌),用涂布棒均匀涂布贴上待测样品,正置15min后将培养皿放置于37℃生化培养箱中倒置培养。培养48h后取出观察培养基上的细菌生长情况并记录抑菌圈直径(D),每组三个平行样。
表2抗菌性能测试结果
由表2试验结果可知本发明制备的含微电池的电活性敷料对金黄色葡萄球菌和大肠杆菌均有明显的抑菌圈,表明含微电池的电活性敷料具有优异的抗菌性能。
Claims (4)
1.一种含微电池的电活性敷料的制备方法,其特征在于:所述方法具体步骤为:
步骤一:将高分子纤维敷料基材置于真空干燥箱中30~105℃下干燥,使其含水量低于0.01%;
步骤二:在步骤一得到的高分子纤维敷料基材表面覆盖Ag限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为Ag靶,真空度为1×10-3~1×10-4Pa,溅射气氛为氧气和氩气的混合气体,氩气流量为15~50sccm,氧气与氩气的通入比例为:1/1~2/1之间,溅射功率为30~100W,溅射时间为15~120min,即得到含有Ag电极圆点阵列的高分子纤维敷料;所述的Ag限域模板上包含直径为1~3mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列;
步骤三:在步骤二得到的含Ag电极微孔阵列的高分子纤维敷料表面覆盖Zn限域模板,然后置于溅射设备真空室,使用直流靶位,选用靶材为Zn靶,真空度为1×10-3~1×10-4Pa,溅射气氛为氩气,氩气流量为15~50sccm,溅射功率为50~130W,溅射时间为15~120min,即得到含微电池的电活性敷料;所述的Zn限域模板上包含直径为0.5~1.5mm,相邻微孔圆心距为2~6.5mm的电极微孔阵列。
2.根据权利要求1所述的一种含微电池的电活性敷料的制备方法,其特征在于:步骤一中,所述的高分子纤维敷料基材为纤维素纤维、再生纤维素纤维、氧化纤维素纤维、氧化再生纤维素纤维、海藻纤维、壳聚糖纤维、蚕丝纤维、丙纶纤维、聚乙烯醇纤维、聚酯纤维的单一/混纺织物或其非织造物。
3.根据权利要求1所述的一种含微电池的电活性敷料的制备方法,其特征在于:步骤三中,所述的Ag限域模板上的电极微孔阵列的微孔直径始终为Zn限域模板上的电极微孔阵列的微孔直径的1~2倍。
4.根据权利要求3所述的一种含微电池的电活性敷料的制备方法,其特征在于:步骤三所得电活性敷料上Ag电极圆点与相邻的Zn电极圆点之间的圆心距为1~3.25mm。
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