CN111295475B - 具有功能复合粒子的纤维布及其制备方法 - Google Patents
具有功能复合粒子的纤维布及其制备方法 Download PDFInfo
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Abstract
本申请涉及一种具有功能复合粒子的纤维布及其制备方法,所述制备方法包括采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中,经由加热蒸发到真空物理气相沉积PVD工艺炉中冷凝;对冷凝状态下的功能金属粒子的外表面采用PVD工艺沉积PVD陶瓷层,以形成所述功能复合粒子;及将所述功能复合粒子通过粒子筛选器筛选及加速以轰击纤维布,从而将所述功能复合粒子植入所述纤维布中,以形成所述具有功能复合粒子的纤维布。本申请的功能复合粒子能够降低内部功能金属粒子与外界氧气的接触并缓慢的施放功能金属粒子的离子态金属离子,延长了功能金属粒子的作用时间。本申请藉由在纤维布中植入功能复合粒子,从而实现具有长效持久的抗菌效果的纤维布。
Description
本申请要求申请号为PCT/CN2017/093391的PCT专利申请案的优先权,所述PCT专利申请案的全文以引用方式并入本文中。
技术领域
本发明涉及复合材料技术领域,特别涉及具有功能复合粒子的纤维布及其制备方法。
背景技术
以下说明及实例并不由于其包含于此章节中而被认为是现有技术。
抗菌干巾或布料的制备方法一般是通过两种技术方案,第一种技术方案是将抗菌材料制成丝线(银线或铜线)织入纤维布料中,第二种技术方案是将抗菌材料制成抗菌粒子并通过喷涂,印染,或PVD技术,将抗菌粒子覆涂在纤维布料表面,从而使纤维布料有抗菌功能。
然而,第一种技术方案的缺陷是成本昂贵,纤维布料表面抗菌性能不均匀。而第二种技术方案由于将抗菌粒子直接覆涂在纤维布料表面,会造成抗菌粒子直接长时间与空气接触,表面形成氧化层,无法维持持久长效抗菌。此外,当覆涂在纤维布料表面的抗菌粒子遇到清洗,揉搓等外力作用时,会使得抗菌粒子脱落,进而导致纤维布料失去抗菌效果。
有鉴于此,抗菌干巾或布料的制备方法还有改进的空间。
发明内容
本发明的实施例之一在于提供具有功能复合粒子的纤维布及其制备方法,以试图在至少某种程度上解决至少一种存在于相关领域中的问题。
根据本发明的一实施例,本发明提供了一种制备具有功能复合粒子的纤维布的方法其包含以下步骤:采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中,经由加热蒸发到真空物理气相沉积(PVD)工艺炉中冷凝;随后对冷凝状态下的功能金属粒子的外表面采用PVD工艺沉积PVD陶瓷层,以形成所述功能复合粒子;最后将所述功能复合粒子通过粒子筛选器筛选及加速以轰击纤维布,从而将所述功能复合粒子植入所述纤维布中。
在一些实施例中,所述粒子筛选器包含磁场生成装置、电场生成装置以及档板,其中磁场方向与电场方向大体上垂直。
在一些实施例中,所述电场生成装置为功率为约5Kw-约30Kw的独立偏压电源。
在一些实施例中,所述磁场的大小为约5mT–约1000mT。
在一些实施例中,其中所述电场的大小为约5KV–约60KV。
在一些实施例中,所述纤维布以大体上垂直于所述功能复合粒子的轰击方向的线速度10m/min-40m/min移动。
在一些实施例中,经筛选后的所述功能复合粒子的粒径为约15nm–约500nm,且经筛选后的所述功能复合粒子的能量在约5KeV–约60KeV范围内。
在一些实施例中,所述功能金属粒子是抗菌金属粒子,所述抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
在一些实施例中,所述PVD陶瓷层包括Zr、Ti、Al、V、Nb、Ta、Y、Fe、Cr、Mo、W或其组合所构成的金属氧化物、金属氮化物或其混合物。
在一些实施例中,所述PVD陶瓷层为由ZrN、TiN、AlTiN、Al2O3、ZrO2、TiO2、VN、NbN、TaN、YN、FeN、CrN、MoN、WN、V2O5、Nb2O5、Ta2O5、Y2O3、Fe2O3、Cr2O3、MoO2或WO2构成的PVD陶瓷层。
在一些实施例中,所述纤维布的材料选自棉、麻、丝绸、人造纤维及其组合。
根据本发明的另一实施例,本发明提供一种纤维布,其中所述纤维布的纤维中具有功能复合粒子,其中所述功能复合粒子包括:内核,所述内核由功能金属粒子构成,具有外表面;以及壳层,所述壳层为物理气相沉积(PVD)陶瓷层,所述壳层附着在所述内核的外表面,其中,所述壳层为结晶结构从而允许所述内核中的功能金属粒子的离子态经由晶界缓释至所述壳层外。
在一些实施例中,所述功能复合粒子在所述纤维布中的分布密度为约106个/cm2-约108个/cm2。
本申请实施例的额外层面及优点将部分地在后续说明中描述、显示、或是经由本申请实施例的实施而阐释。
附图说明
在下文中将简要地说明为了描述本申请实施例所需要的附图。显而易见地,下文描述中的附图仅只是本申请中的部分实施例。对本领域技术人员而言,在不需要创造性劳动的前提下,依然可以根据这些附图中所例示的结构来获得其他实施例的附图。
图1所示是根据本发明一实施例的功能复合粒子的结构示意圖;
图2所示是根据本发明一实施例的具有功能复合粒子的纤维布的示意圖;
图3所示是根据本发明一实施例中的功能复合粒子通过粒子筛检器的示意图。
具体实施方式
为更好的理解本发明的精神,以下结合附图和具体实施例对本发明实施例提供的功能复合粒子作进一步详细说明。根据以下说明及权利要求书,本发明实施例的优点和特征将更清楚。
如本文中所使用,术语“大致”、“大体上”、“实质”及“约”用以描述及说明小的变化。当与事件或情形结合使用时,所述术语可指代其中事件或情形精确发生的例子以及其中事件或情形极近似地发生的例子。举例来说,当结合数值使用时,术语可指代小于或等于所述数值的±10%的变化范围,例如小于或等于±5%、小于或等于±4%、小于或等于±3%、小于或等于±2%、小于或等于±1%、小于或等于±0.5%、小于或等于±0.1%、或小于或等于±0.05%。举例来说,如果两个数值之间的差值小于或等于所述值的平均值的±10%(例如小于或等于±5%、小于或等于±4%、小于或等于±3%、小于或等于±2%、小于或等于±1%、小于或等于±0.5%、小于或等于±0.1%、或小于或等于±0.05%),那么可认为所述两个数值“大体上”相同。
需说明的是,图1-3中的示意图采用简化形式且使用非精准比例,仅用以方便、明晰地辅助说明本发明实施例。
图1展示了根据本发明一实施例的功能复合粒子的结构示意图,其中,功能复合粒子10包括内核11和壳层12,其中内核11由功能金属粒子构成,具有外表面111。壳层12附着在内核11的外表面111上,是一种由陶瓷材料构成的物理气相沉积(PVD)陶瓷层。
图2展示了本发明一实施例所提供的一种具有功能复合粒子的纤维布的示意图,所述纤维布20是通过带电粒子注入方法,将上述实施例中的功能复合粒子10,植入到所述纤维布20的纤维内部。由图1和图2可看出,所述功能复合粒子10位于纤维布20内的纤维聚合大分子所形成的缝隙和孔洞中,其中所述功能复合粒子中的壳层12为结晶结构并具有晶界121,该晶界121为内核11中的功能金属粒子的离子态提供了通向壳层12外部的通道。在本发明一实施例中,在该功能复合粒子10的使用过程中,由于壳层为结晶结构,内核11中的功能金属粒子可以以离子态的形式经由晶界121缓慢释放到壳层12的外部。此外,包裹在内核11外表面111的壳层12可以有效阻止内核11中的功能金属粒子与外界的氧气接触,避免其过早地被氧化。通过以离子态的形式缓慢释放所述功能金属粒子以及降低所述功能金属粒子与外界氧气的接触,延长了功能金属粒子的作用时间,从而实现具有长效持久的抗菌效果的纤维布。
为了获得上述具有功能复合粒子的纤维布,本发明一实施例提供了一种制备具有功能复合粒子的纤维布的方法,具体包括以下步骤:首先,采用蒸发冷凝工艺将功能金属粒子的固体金属块体放入坩埚中,经由加热蒸发到真空物理气相沉积(PVD)工艺炉中冷凝,以形成内核11;随后对冷凝状态下的功能金属粒子的外表面111采用PVD工艺沉积由陶瓷材料构成的壳层12,以形成功能复合粒子10。随后,将所述功能复合粒子在真空炉中经过粒子筛选器以对所述功能复合粒子筛选及加速以轰击纤维布,从而将所述功能复合粒子植入所述纤维布中。
在本发明的一实施例中,功能金属粒子冷凝后的粒径受加热源加热功率的影响。
在本发明的一实施例中,使用电子枪作为加热源来加热功能金属粒子组成的固体金属块体,电子枪的电流强度范围为约60A-300A。
在本发明的一实施例中,采用PVD工艺形成PVD陶瓷层的步骤包括:在真空物理气相沉积PVD工艺炉中通入纯度为约99.999%的氮气或氧气,在偏压为约0V-1000V的条件下,打开包含生物可相容陶瓷材料的靶,弧电流为约120A-200A,采用PVD工艺将冷凝状态下的功能金属粒子的外表面沉积PVD陶瓷层。
本发明实施例可通过常规的PVD设备采用常规的PVD工艺形成壳层12。
在本发明一实施例中,所述功能复合粒子10的粒径范围为约15nm–约50000nm。在本发明的一实施例中,所述功能金属粒子是抗菌金属粒子,所述抗菌金属粒子包括Ag金属粒子、Cu金属粒子、Zn金属粒子或其混合物。在本发明的一实施例中,壳层12为由Zr、Ti、Al、V、Nb、Ta、Y、Fe、Cr、Mo、W或其组合所构成的金属氧化物、金属氮化物或其混合物构成的物理气相沉积陶瓷层,其厚度为约5nm–约20000nm,表面硬度为1000HV-4500HV,较佳为3000HV-4000HV。在本发明的一实施例中,壳层12为由ZrN、TiN、AlTiN、Al2O3、ZrO2、TiO2、VN、NbN、TaN、YN、FeN、CrN、MoN、WN、V2O5、Nb2O5、Ta2O5、Y2O3、Fe2O3、Cr2O3、MoO2或WO2构成的物理气相沉积陶瓷层。
申请号为PCT/CN2017/093391的PCT专利申请案中例示了数种功能复合粒子10的具体实施例,其全文以引用方式并入本文中。
在本发明一实施例中,所述粒子筛检器包括磁场生成装置、电场生成装置以及档板,其中磁场方向与电场方向大体上垂直。
图3所示是根据本发明一实施例中的功能复合粒子通过粒子筛检器的示意图。如图3所示,在本发明一实施例中,所述粒子筛选器30包括生成磁场B的磁场生成装置、生成电场E的电场生成装置以及具有开口31的档板。本领域技术人员应可清楚理解,虽然图3中磁场B的方向(垂直进入纸面方向)显示与电场E的方向垂直,实际操作中,两者间的夹角存在些许误差是可以允许的,不必然是完美的90度。此外,所述生成磁场B的磁场生成装置包含任何可以生成磁场的装置,举例来说,所述装置可以是,但不限于,强磁铁或其他电磁装置。所述生成电场E的电场生成装置包含任何可以生成电场E的装置。在本发明的一实施例中,所述电场装置可以包括,但不限于,独立偏压电源,其中所述独立偏压电源的功率为约5Kw-约30Kw。在本发明的一实施例中,所述磁场B的大小为约5mT–约1000mT。在本发明的一实施例中,所述电场的大小为约5KV–约60KV。在本发明的一实施例中,所述磁场为定向均匀的磁场,所述电场为定向均匀的电场。
所述功能复合粒子形成后由于带有少量电荷,因此,注入所述粒子筛选器30时能够沿著电场E的方向加速移动;与此同时磁场B提供一个大体上垂直于所述功能复合粒子的移动方向的向心力(也称作洛伦兹力),从而使所述功能复合粒子的运动轨迹发生变化(如图3中虚线T所示)。
向心力F的大小可通过以下公式计算:F=BQV=MV2/R(1),由公式(1)可知当通过调整电场E及磁场B使粒子速度V及磁场B皆为固定的情况下,粒子的运动半径R(即运动轨迹)与粒子的质量M(粒子粒径)成正比并与其所带电荷Q成反比,通过在所述档板上设置与磁场B的方向大体上平行的开口31,所述开口31可以使具有特定运动轨迹的所述功能复合粒子通过所述粒子筛选器30并阻挡其他功能复合粒子。因此,只有质量M(粒子粒径)和带电荷Q(能量)在合适范围内的所述功能复合粒子才能通过所述粒子筛检器。
在本发明一实施例中,所述开口31的开口大小为约1cm-约2cm。在本发明一实施例中,通过调整外加磁场B和电场E的数值,可以调整通过加速器粒子的粒径和能量,从而进行所述功能复合粒子的筛选。
本申请实施例提供的具有功能复合粒子的纤维布及其制备方法具有以下的特点及优势:
由于一般纤维布中的纤维的粒径在约10um-100um的范围内,举例来说,棉布纤维的粒径为约38um-51um、毛型纤维的粒径为约64um-114um以及人造纤维的粒径为约30um-50um,且纤维布中的纤维是由有序的晶态结构和无序的非晶态结构组成的混合物。在非晶态结构中,纤维布中的纤维的大分子排列比较混乱,堆砌比较疏松,有较多的缝隙空洞。在本发明一实施例中,通过调整所述粒子筛选器中的电场E与磁场B的强度,以使通过所述筛选器筛选及加速的所述功能复合粒子的粒径为约15nm–约500nm,且其能量在约5KeV–约60KeV范围内,进而使通过所述粒子筛选器的所述功能复合粒子轰击所述纤维布时,所述功能复合粒子能够穿过所述纤维布中的纤维大分子的表面势垒,并通过所述纤维布内的非晶态结构的缝隙孔洞,从而植入所述纤维布的内部,并和所述纤维布中的纤维大分子经过一系列碰撞后,牢牢地镶嵌在所述纤维中。在本发明一实施例中,通过所述筛选器筛选及加速的所述功能复合粒子的粒径为约15nm–约100nm。
在本发明一实施例中,经过碰撞后,所述功能复合粒子能量大部分转化为纤维的弹性势能和少部分热能,由于入射的所述功能复合粒子的粒径远远小于所述纤维布的所述纤维的粒径,所述功能复合粒子引起的弹性形变远远小于所述纤维的弹性极限,因此不会造成所述纤维布的物理性能产生变化。
在本发明一实施例中,可通过调整所述电场生成装置的功率大小来控制所述功能复合粒子的入射粒子流密度,同时设置纤维布以特定的速度运动前移,从而控制单位面积内植入纤维布中的功能复合粒子的密度。藉由将单位面积内植入纤维布中的功能复合粒子的密度控制在合理的范围内,使得纤维布有优秀的抗菌效果的同时,又不会使纤维布因功能复合粒子过多积累热量,造成纤维布软化变形。
在本发明一实施例中,所述纤维布以大体上垂直于所述功能复合粒子的轰击方向的线速度10m/min-40m/min移动。在本发明一实施例中,所述功能复合粒子在所述纤维布中的分布密度为约106个/cm2-约108个/cm2。
在本发明一实施例中,所述功能复合粒子可植入到任意材料的纤维布中,举例来说,所述纤维布的材料可以选自,但不限于,棉、麻、丝绸,和人造纤维中的一种或多种。
以下结合本发明具体的较优实施例以进一步说明本发明具有功能复合粒子的纤维布的制备。
实施例1
首先,将Ag银金属块放入坩埚中,并采用电子枪以电流强度100A加热Ag银金属块以使其蒸发到保持在真空下的物理气相沉积PVD工艺炉中冷凝,从而形成冷凝状态下的Ag银金属粒子;
之后在真空的物理气相沉积PVD工艺炉中导入纯度为99.999%的氮气,通过偏压大小为90V的条件下,打开包含Ti的靶,以弧电流为150A,对所述冷凝状态下的Ag银金属粒子的外表面采用PVD工艺以沉积TiN陶瓷层,从而形成带电的功能复合银粒子;
随后将带有电荷的功能复合银粒子导入粒子筛选器中,其中所述粒子筛选器的磁场大小为约700mT,而其独立偏压电源的功率为10Kw,以形成约20KV的电场大小,使得通过粒子筛选器的功能复合银粒子的粒径为约50nm–约70nm,且其能量在约5KeV–约60KeV范围内;将棉质材料的纤维无纺布放置于离粒子筛选器开口处,使纤维无纺布的表面大体上垂直于粒子射出方向,并以30m/min的线速度使纤维无纺布的表面经过粒子筛选器的开口,从而使功能复合银粒子均匀的打入纤维无纺布的表面上,以形成粒子分布密度为约107个/cm2的具有功能复合银粒子的纤维无纺布。
实施例2
首先,将Cu铜金属块放入坩埚中,并采用电子枪以电流强度130A加热Cu铜金属块以使其蒸发到保持在真空下的物理气相沉积PVD工艺炉中冷凝,从而形成冷凝状态下的Cu铜金属粒子;
之后在真空的物理气相沉积PVD工艺炉中导入纯度为99.999%的氮气,通过偏压大小为120V的条件下,打开包含Ti的靶,以弧电流为150A,对所述冷凝状态下的Cu铜金属粒子的外表面采用PVD工艺以沉积TiN陶瓷层,从而形成带电的功能复合铜粒子;
随后将带有电荷的功能复合铜粒子导入粒子筛选器中,其中所述粒子筛选器的磁场大小为约400mT,而其独立偏压电源的功率为15Kw,以形成约13KV的电场大小,使得通过粒子筛选器的功能复合铜粒子的粒径为约45nm–约80nm,且其能量在约5KeV–约60KeV范围内;将棉质材料的纤维无纺布放置于离粒子筛选器开口处,使纤维无纺布的表面大体上垂直于粒子射出方向,并以30m/min的线速度使纤维无纺布的表面经过粒子筛选器的开口,从而使功能复合铜粒子均匀的打入纤维无纺布的表面上,以形成粒子分布密度为约107个/cm2的具有功能复合铜粒子的纤维无纺布。
实施例3
首先,将Zn锌金属块放入坩埚中,并采用电子枪以电流强度80A加热Zn锌金属块以使其蒸发到保持在真空下的物理气相沉积PVD工艺炉中冷凝,从而形成冷凝状态下的Zn锌金属粒子;
之后在真空的物理气相沉积PVD工艺炉中导入纯度为99.999%的氮气,通过偏压大小为70V的条件下,打开包含Ti的靶,以弧电流为150A,对所述冷凝状态下的Zn锌金属粒子的外表面采用PVD工艺以沉积TiN陶瓷层,从而形成带电的功能复合锌粒子;
随后将带有电荷的功能复合锌粒子导入粒子筛选器中,其中所述粒子筛选器的磁场大小为约450mT,而其独立偏压电源的功率为12Kw,以形成约15KV的电场大小,使得通过粒子筛选器的功能复合锌粒子的粒径为约65nm–约90nm,且其能量在约5KeV–约60KeV范围内;将棉质材料的纤维无纺布放置于离粒子筛选器开口处,使纤维无纺布的表面大体上垂直于粒子射出方向,并以30m/min的线速度使纤维无纺布的表面经过粒子筛选器的开口,从而使功能复合锌粒子均匀的打入纤维无纺布的表面上,以形成粒子分布密度为约107个/cm2的具有功能复合锌粒子的纤维无纺布。
上文说明摘要整理出数个实施例的特征,这使得所属技术领域中具有通常知识者能够更加理解本申请的多种方面。所属技术领域中具有通常知识者可轻易地使用本申请作为基础,以设计或修改其他组合物,以便实现与此处申请的实施例相同的目的及/或达到相同的优点。所属技术领域中具有通常知识者亦可理解,这些均等的实例并未悖离本申请的精神与范畴,且其可对本申请进行各种改变、替换与修改,而不会悖离本申请的精神与范畴。虽然本文中所揭示的方法已参考以具体次序执行的具体操作加以描述,但应理解,可在不脱离本申请的教示的情况下组合、细分或重新排序这些操作以形成等效方法。因此,除非本文中特别指示,否则操作的次序及分组不是对本申请的限制。
Claims (16)
1.一种制备具有功能复合粒子的纤维布的方法,其包含:
采用蒸发冷凝工艺将由功能金属粒子组成的固体金属块体放入坩埚中,经由加热蒸发到真空物理气相沉积PVD工艺炉中冷凝;
对冷凝状态下的功能金属粒子的外表面采用PVD工艺沉积PVD陶瓷层,以形成所述功能复合粒子;及
将所述功能复合粒子通过粒子筛选器筛选及加速以轰击纤维布,从而将所述功能复合粒子植入所述纤维布中,其中所述粒子筛选器包含磁场生成装置、电场生成装置以及档板,其中磁场方向与电场方向大体上垂直,其中经筛选后的所述功能复合粒子的粒径为15nm–500nm,且经筛选后的所述功能复合粒子的能量在5KeV–60KeV范围内。
2.根据权利要求1所述的方法,其中所述电场生成装置为功率为5Kw-30Kw的独立偏压电源。
3.根据权利要求1所述的方法,其中所述磁场的大小为5mT–1000mT。
4.根据权利要求1所述的方法,其中所述电场的大小为5KV–60KV。
5.根据权利要求1所述的方法,其中所述纤维布以大体上垂直于所述功能复合粒子的轰击方向的线速度10m/min-40m/min移动。
6.根据权利要求1所述的方法,其中所述功能金属粒子是抗菌金属粒子,所述抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
7.根据权利要求1所述的方法,其中所述PVD陶瓷层包括Zr、Ti、Al、V、Nb、Ta、Y、Fe、Cr、Mo、W或其组合所构成的金属氧化物、金属氮化物或其混合物。
8.根据权利要求7所述的方法,其中所述PVD陶瓷层为由ZrN、TiN、AlTiN、Al2O3、ZrO2、TiO2、VN、NbN、TaN、YN、FeN、CrN、MoN、WN、V2O5、Nb2O5、Ta2O5、Y2O3、Fe2O3、Cr2O3、MoO2或WO2构成的PVD陶瓷层。
9.根据权利要求1所述的方法,其中所述纤维布的材料选自棉、麻、丝绸、人造纤维或其组合。
10.一种根据权利要求1-9中任一权利要求所述的方法制成的纤维布,其中所述纤维布的纤维中具有功能复合粒子,其中所述功能复合粒子包括:
内核,所述内核由功能金属粒子构成,具有外表面;以及
壳层,所述壳层为物理气相沉积PVD陶瓷层,所述壳层附着在所述内核的外表面,
其中,所述壳层为结晶结构从而允许所述内核中的功能金属粒子的离子态经由晶界缓释至所述壳层外。
11.根据权利要求10所述的纤维布,其中所述功能金属粒子是抗菌金属粒子,所述抗菌金属粒子是Ag金属粒子、Zn金属粒子、Cu金属粒子或其混合物。
12.根据权利要求10所述的纤维布,其中所述PVD陶瓷层包括Zr、Ti、Al、V、Nb、Ta、Y、Fe、Cr、Mo、W或其组合所构成的金属氧化物、金属氮化物或其混合物。
13.根据权利要求12所述的纤维布,其中所述PVD陶瓷层为由ZrN、TiN、AlTiN、Al2O3、ZrO2、TiO2、VN、NbN、TaN、YN、FeN、CrN、MoN、WN、V2O5、Nb2O5、Ta2O5、Y2O3、Fe2O3、Cr2O3、MoO2或WO2构成的PVD陶瓷层。
14.根据权利要求10所述的纤维布,其中所述功能复合粒子的粒径为15nm–500nm。
15.根据权利要求10所述的纤维布,其中所述功能复合粒子在所述纤维布中的分布密度为106个/cm2-108个/cm2。
16.根据权利要求10所述的纤维布,其中所述纤维布的材料选自棉、麻、丝绸、人造纤维或其组合。
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