CN105517973A - 装置和方法 - Google Patents
装置和方法 Download PDFInfo
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- CN105517973A CN105517973A CN201480049374.0A CN201480049374A CN105517973A CN 105517973 A CN105517973 A CN 105517973A CN 201480049374 A CN201480049374 A CN 201480049374A CN 105517973 A CN105517973 A CN 105517973A
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61M1/00—Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
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Abstract
我们描述了一种制造具有受控过滤器通道开口尺寸的陶瓷过滤器的方法,所述方法包括:制造陶瓷前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含陶瓷材料;以及烧结所述陶瓷前体元件以使所述陶瓷材料融合并且移除所述聚合物材料;所述方法还包括移除所述第一表面的受控厚度部分以使所述呈喇叭形展开的孔开口至所述受控过滤器通道开口尺寸。
Description
发明领域
本发明涉及制造陶瓷过滤器的方法,涉及由这样的方法制造的过滤器,并且涉及结合这样的过滤器的医疗器械。
发明背景
已知使用径迹蚀刻(track-etch)技术由薄塑料膜制造过滤器,用带电粒子轰击膜并且随后进行化学蚀刻。另一种技术使用激光束在聚合物膜中钻孔。第三种方法是采用光刻。然而,这些过滤器倾向于是易坏的、昂贵的并且对于许多应用不适用。
原则上,陶瓷材料应当是对微滤有利的,但是不存在容易的制造所需孔径的技术。
背景现有技术可以发现于:
US6479099B |
US5340779A |
EP1020276A |
US2004091709A |
US2002074282A |
WO03072233A |
US2007142208A |
US2011100910A |
US2008022644A |
US2007119135A |
US4746341A |
US2006192326A |
KR100445768B |
另外的背景现有技术可以发现于:“Al2o3、Al2o3-Sio2和Al2o3-高岭土中空纤维膜的制备、表征和渗透性质(Preparation,CharacterizationAndPermeationPropertyOfAl2o3,Al2o3-Sio2AndAl2o3-KaolinHollowFiberMembranes)”,Han等人,JournalOfMembraneScience,372卷,1-2期,2011年4月15日,154-164页;以及“用于从水中高效吸收聚芳族烃的混合超支化聚合物/陶瓷过滤器的优化(OptimizationOfHybridHyperbranchedPolymer/CeramicFiltersForTheEfficientAbsorptionOfPolyaromaticHydrocarbonsFromWater)”,TsetsekouA等人,JournalOfMembraneScience,311卷,1-2期,2008年3月20日,128-135页。
发明概述
根据本发明,因此提供了一种制造具有受控过滤器通道开口尺寸的陶瓷过滤器的方法,所述方法包括:制造陶瓷前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含陶瓷材料;以及烧结所述陶瓷前体元件以使所述陶瓷材料融合并且移除所述聚合物材料;所述方法还包括移除所述第一表面的受控厚度部分以使所述呈喇叭形展开的孔开口至所述受控过滤器通道开口尺寸。
在实施方案中,通过将掺杂剂(dope)形成为元件所需的形状来制造陶瓷前体元件,所述掺杂剂包含陶瓷材料、聚合物、和用于聚合物的溶剂。之后在其中溶剂(但不是聚合物)可溶混的液体浴中处理所形成的形状。例如,可以采用与水性(水)浴组合的极性溶剂。一般来说,在处理期间,以形成对流单体的方式在浴中用液体(水)代替溶剂,留下在前体元件的表面之间延伸的大体上锥形的孔的基本上规则的排列。原则上,可以采用除陶瓷材料外的无机材料。如果元件包括非常薄的膜,呈喇叭形展开的孔的顶点不完全达到第一表面,尽管在实施方案中它们可以正好与该表面相交,留下非常小的孔,例如小于0.1μm。在灼烧期间,将聚合物材料烧尽,在烧结的陶瓷中留下呈喇叭形展开的孔。之后通过从第一表面移除材料的受控厚度层,可以将呈喇叭形展开的孔打开至所需的程度。
在实施方案中,前体元件可以包括材料的薄片或膜、或材料的管。可以通过将溶剂沉积至该表面上(优选与在陶瓷前体中相同的种类(极性的或非极性的)),并且留下溶剂以溶解第一表面的薄层,任选通过振荡辅助,来移除第一表面的一部分。例如,可以将溶剂倾倒至膜的顶部或者可以将管状纤维浸入至溶剂中。将溶剂留下例如约1分钟至约24小时的时间段,通过将陶瓷前体放置到用于烧结的烘箱中停止溶解过程。
另外地或备选地,可以例如,借助受控高度切割器如在可调节导螺杆上的刀片,物理移除陶瓷前体元件的第一表面的一部分——这样的布置通常可以将被移除的材料的厚度控制为好于1μm。在烧结之前,该过程可以干燥进行或者利用润滑剂进行。在烧结之后,通过例如使用可控高度旋转研磨盘如金刚石抛光机研磨,或者通过采用利用与过滤器中陶瓷材料类似的材料的陶瓷粒子(例如,微米尺度或亚微米尺度氧化铝粒子、金刚石、和/或氧化硅)的砂纸状研磨工艺,可以将材料移除。在另一种方法中,可以使用光纤抛光膜(lappingfilm)研磨表面;这可以采用多种材料,如氧化硅、金刚石、氧化铝、二氧化钛、等。
本发明还提供一种陶瓷过滤器,所述陶瓷过滤器具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸并且与所述第一和第二表面连接的呈喇叭形展开的通道的排列。
在实施方案中,陶瓷前体中的锥形孔全部为基本上相同的尺寸并且在顶点具有基本上相同的夹角。因此,通过从第一表面移除材料,可以准确地控制孔的尺寸——尽管在实施中,我们描述的技术的实施方案倾向于对孔的开口的最大尺寸(直径)设置上限——这对于过滤器来说是有用的性质。
过滤器结构的实施方案具有呈喇叭形展开的通道,其可用于降低阻塞/阻挡的风险。典型的过滤器孔直径在0.1-20μm的范围内,尽管可以制造较大的孔(受在第二表面的孔的尺寸限制,其取决于元件的厚度)。因此,在通过该过程制造的过滤器的实施方案中,呈喇叭形展开的通道是大体上圆形的并且多于90%具有大于0.1μm、0.2μm、0.5μm或1μm的直径(在一端或两端)。在实施方案中,通道的开口可以具有小于100μm、50μm、30μm、20μm、10μm、5μm或2μm的直径(在一端或两端)。这是可用的,因为难以通过其他技术可靠地制造这样的孔径。
通过上述技术制造的过滤器的一个有利的应用是分离血液组分,尤其是将红细胞与其他血液组分分离。例如,血小板可以具有小于1μm的直径,红细胞可以具有大约7μm的尺寸,并且白细胞以及血液中的其他细胞如干细胞可以具有在10-20μm的范围内的尺寸。因此,通过选择小于5μm、4μm、3μm或2μm的孔径(可以将红细胞挤压通过小至1-3μm的孔),可以制造白细胞去除(leukoreduction)过滤器。常规血液过滤装置在过滤过程中可能会损失约5-10%的红细胞,但是结合了我们已经描述的类型的陶瓷过滤器的血液过滤装置可以是基本上更高效的。此外,提高了残留物的质量并且可以回收残留物以提取材料如干细胞或白细胞,例如用于研究。
尽管我们已经描述的技术的实施方案尤其可用于制造具有受控孔径的过滤器,它们可以更通常用于制造陶瓷过滤器元件而不必须控制孔径,并且可能地,采用除陶瓷材料外的其他无机材料。
因此,在另一个方面中,本发明提供一种制造无机过滤器的方法,所述方法包括:制造前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含无机材料;以及烧结所述前体元件以使所述无机材料融合并且移除所述聚合物材料;所述方法还包括移除所述第一表面的一部分以使所述呈喇叭形展开的孔开口。
之前描述的技术均可以用于本发明的这个方面的实施方案中。尤其是,可以在烧结之前和/或烧结之后,尤其是使用之前描述的技术物理和/或化学移除第一表面的一部分。以这种方式制造的过滤器同样通常可以用于,例如血液过滤装置或细胞分离。
在制造过程的典型实施方案中,在第二表面上留下薄的(例如2-3μm)蒙皮(skin)。在存在的情况下,这可以在烧结之前或之后通过如上所述的方法移除以制造过滤器结构。备选地,可以将其留在适当位置以使得能够制造一组可控孔的呈喇叭形展开的孔。
因此,在本发明的另一个方面中,提供一种陶瓷板,所述陶瓷板具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸并且与所述第一和第二表面连接的呈喇叭形展开的通道的排列,以限定一组呈喇叭形展开的孔。还提供了制造这样的板的方法。
原则上,过滤器结构可以具有除过滤外的应用。例如,可以例如通过选择性研磨将一个或两个表面图案化,并且图案化结构可以用作针对可见光或非可见光的罩。可以例如通过CNC刳刨机(router)进行这样的选择性研磨。该类型的罩可以用于,例如显示标志,或者可能地,与较小尺度的图案一起使用,作为光刻的罩。
因此本发明还提供制造具有受控通道开口尺寸的陶瓷板的方法,更具体地是制造罩的方法,所述方法包括:制造陶瓷前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含陶瓷材料;以及烧结所述陶瓷前体元件以使所述陶瓷材料融合并且移除所述聚合物材料;所述方法还包括移除所述第一表面的受控厚度部分以使所述呈喇叭形展开的孔开口至所述受控通道开口尺寸。
本发明还提供具有包括第一和第二表面的板/罩结构以及在所述第一和第二表面之间延伸并且与所述第一和第二表面连接的呈喇叭形展开的通道的排列,任选地,其中将板/罩结构的呈喇叭形展开的通道的排列图案化。
在上述制造方法/过滤器/平板/结构的实施方案中,可以处理过滤器的表面以改变表面的物理、化学或生物特性,尤其是提供具有表面涂层的过滤器。例如,可以等离子体处理表面,也就是说,使得表面亲水或疏水,和/或可以用分子材料处理表面以使表面功能化。在实施方案中,涂布过滤器的表面以改变过滤特性,尤其是更有效地选择或过滤一个或多个靶标。
本发明还提供使用如上所述/如由上述方法制造的过滤器从流体(液体或气体)中过滤粒子的方法。
附图简述
现在将仅通过实例的方式,参照附图,进一步描述本发明的这些和其他方面,其中:
图1a和1b示意性地示出了在根据本发明的实施方案制造陶瓷过滤器的方法中的孔径控制的原理,以及以这种方式制造的过滤器的实施方案的顶部和底部的示意图;
图2a和2b分别示出了纤维前体元件的制造和膜/圆片前体元件的制造;
图3示意性地示出了通过水浴处理的膜前体元件的垂直横截面;
图4示出了可以用于从陶瓷前体元件中移除层的受控高度切割器的实例;
图5a和5b图示了圆形陶瓷元件,以及金刚石抛光机用于研磨烧结的陶瓷元件的用途;
图6示意性地图示了使用根据本发明的实施方案的陶瓷过滤器的血液过滤;
图7示出了根据本发明的膜过滤器的实施方案的粒子分离的范围(标记为“微滤”),连同用于不同粒径的其他分离原理;
图8示出了根据本发明的实施方案的陶瓷过滤器在显微镜下的顶视图的图像(100x的放大率),以及用于提供沿着所示出的膜表面的长度具有不同开口尺寸的孔的跨过滤器的顶部的对角线切割的示意图;和
图9示出了一组使用根据本发明的实施方案的方法制造的功能性过滤器的图像,其示出了:9a)膜的横截面图(100x的显微镜放大率);9b)膜在研磨顶部表面之后的顶视图(100x的显微镜放大率);9c)图9b中的膜在进一步研磨顶部表面之后的顶视图(100x的显微镜放大率);9d)膜在研磨底部表面之后的底视图(100x的显微镜放大率);和9e)根据所描述的方法制备的膜过滤器的顶部的透视图(盘直径50mm)。
优选实施方案详述
用于由溶胶-凝胶流延(casting)制造陶瓷材料的技术包括制造掺杂剂溶液,其由粘合剂(或分散剂)、所述粘合剂可溶于其中的溶剂以及晶体形式的陶瓷材料(如,但不限于,氧化铝、氧化锆等)组成。这些制造了高度组织化的内部孔。我们采用了改进的这样的结构,用于在微米范围(0.1μm-100μm)内微滤粒子。过滤器的优势包括归因于所使用的稳定材料的稳健性(robustness)、低价格、和简单的制造过程。应用包括例如在高温和/或高压和/或酸性或碱性条件存在的情况下,发酵培养液和溶剂提取物的处理、藻酸盐的加工、致热原(pyrogen)和细菌移除、抗生素的制备等。我们还将描述它们用于血液过滤的用途。尤其是,我们将会描述用于在膜上制造所需孔径以使其针对特定微滤应用而调节的技术。
如在图1中所示,通过我们描述的技术的实施方案得到的陶瓷膜过滤器100由锥形孔102构成,其从上到下穿过这些膜104。利用这种孔几何形状,可以通过大批量(其降低了制造成本)制造膜104来实现不同孔径分布的膜104的制造,之后针对预期的应用调整孔102——即具有可变的孔径。这样的方法允许时间和成本需求的减少以开发定制的过滤器-通过改变例如掺杂剂溶液比率、非溶剂的类型、烧结过程的温度、膜104的干燥时间、过滤器100的厚度等,人们可以改变孔角度/填充密度和其他过滤器参数。
因此,我们描述了陶瓷过滤器100中定制的孔径的制造,允许它们用于微滤领域中,尤其是细胞的过滤中的大范围的应用。
最初,用溶剂、陶瓷系材料、和聚合物的混合物制备掺杂剂溶液。
溶剂可以是,但不限于:二甲基甲酰胺、二甲亚砜、二甲基甲酰胺、二甲基乙酰胺、N-甲基-2-吡咯烷酮、六甲基磷酰胺、二烷、衍生自它们的其他溶剂或可以溶解聚合物的可用的其他有机溶剂。
陶瓷系材料可以是,但不限于:氧化铝、氧化钛、氧化锆、碳化硅、玻璃材料、或任何其他类似材料,其任选地用交联剂表面处理。
聚合物材料可以是,但不限于:聚酰胺、聚(己内酯)、聚氨酯、聚(L-乳酸-共-羟基乙酸)、聚丙烯腈、聚酰亚胺、聚(甲基丙烯酸甲酯)、聚(D,L-乳酸酯)、聚苯乙烯、聚醚醚酮、聚醚砜、聚偏二氟乙烯、聚砜、聚醚砜或任何其他类似材料,其优选地用交联剂表面处理。聚合物在掺杂剂中起粘合剂的作用;它应当在烧结温度(600-1500℃)下烧尽(burntaway)。
任选地,可以将分散剂/表面活性剂加入至混合物中。分散剂可以是,但不限于:烷基苯磺酸盐、木质素磺酸盐、脂肪醇乙氧基化物、烷基苯酚乙氧基化物、PEG30二聚羟基硬脂酸酯、硬脂酸钠、4-(5-十二烷基)苯磺酸盐、十二烷基硫酸钠、西曲溴铵、含氟表面活性剂、硅氧烷表面活性剂、烷基醚、聚乙二醇和聚丙二醇的嵌段共聚物、衍生自它们的其他分散剂、和/或任何其他两亲性化合物。
在实例实施方案中,溶剂是二甲亚砜、陶瓷是氧化铝、聚合物是聚醚砜,并且分散剂是PEG30二聚羟基硬脂酸酯。
之后使用流延刀(castingknife)或其他方法控制流延涂层的厚度,将掺杂剂溶液流延至光滑表面。可以因此根据所制造的陶瓷前体元件的所需形状来调节流延掺杂剂溶液的形状。之后立刻将流延掺杂剂溶液转移至水浴中并且在那里静置长于5分钟的时间段,通常过夜,以固化(set)。在该过程期间,溶剂逐渐被水代替,在表面的表面张力作用和对流引起锥形含聚合物区域的基本上常规图案的形成。聚合物和/或聚合物/陶瓷材料混合物基本上不溶于水浴。之后将膜从水中移除并且使其干燥长于5分钟的时间段,例如24小时。
图2a示出了水浴106中的管状前体膜104;图2b示出了形成管状前体元件104的过程。图3示出了在水浴中处理之后的图2a和b的膜104的横截面——PES在烧结期间烧尽。通常,膜可以为约50μm厚度。
更详细地,如在图2a中所示,将包含陶瓷系材料、聚合物和溶剂的掺杂剂溶液108放置到水浴106中。在这个实例中,前体元件104具有直径为300-1000μm并且壁厚度为20-30μm的筒形。应该理解的是,前体元件104可以是任何形状的,其可以由陶瓷膜过滤器100的具体用途而确定。
图2b示出了其中前体元件104具有板状形状的实例。可以在允许在其上形成光滑前体元件104的光滑金属层112上制备前体元件104。如在图2b中所示,可以用光滑玻璃或允许制备光滑前体元件104的其他适合支持体代替金属层112。
可以看出,当将前体元件104放置到水浴106中时,水渗透至前体元件104中并且代替释放至水浴106中的溶剂110。如以上概述的,可以将前体元件104置于水浴106中长于5分钟的时间段。
图3示出了根据图2b中图示的而制备的前体元件104的横截面图。可以看出,在要制造孔102的区域中,形成了水和聚合物的混合物114。
为了从前体元件104中移除水/聚合物混合物114,首先从水浴106中移除膜并且之后静置干燥预定量的时间。之后,可以通过在预定温度烧结将聚合物烧尽,在这个实例中所述温度为600-1500℃之间。
在形成前体元件104之后,使用工具400,如流延刀或其他类似装置(图4)通过刮擦(scrapping)表面并且移除在0μm至膜104的最终厚度之间的厚度来移除膜104的顶层。要被刮擦掉的膜104的层的厚度可通过用于刮擦的工具400控制。该过程也可以通过以下方式完成:将溶剂(来自上述清单)倾倒在膜的顶部上并且使其在膜的顶部静置通常长于1秒的时间段,或者将其振荡以加速该过程,使用上述相同的方法将膜的表面刮擦至洁净并且立刻进行膜的烧结。
之后将膜切成所需的过滤器形状,例如圆形,如在图5a中所示。这可以使用圆形刀完成。之后烧结膜,例如在高于600摄氏度的温度烧结约为两小时的时间段,接着在1200-1600摄氏度烧结至少1小时(例如3-4小时)。之后,根据时间、压力和所使用的研磨材料,任选地通过研磨膜的表面进一步处理膜过滤器,以使得其孔更大。图5b示出了通过在边缘的固定件504固定在适当位置的过滤器100的中心、活性区域502的抛光。在这个实例中,将金刚石抛光工具506置于过滤器100的中心、活性区域502的顶部。金刚石抛光工具506具有圆形盘的形状,并且如图示围绕其自身的轴旋转以在活性区域502中研磨过滤器100的表面。技术人员将会理解,经由工具506施加至活性区域502的压力、金刚石抛光工具506的粗糙度和磨耗度、旋转速度、和其他参数可以决定研磨速率。将理解的是,可以用另一种用于研磨活性区域502的适合的材料代替金刚石抛光机。如在图5b中所示,金刚石抛光工具506可以是在垂直方向上可控的,从而限定在要被研磨的活性区域502上的材料的量。
因此,两个主要的选择可用于控制孔径:过程1)在膜104的流延之后并且在膜104的烧结之前;和过程2)在膜104的烧结之后,已经获得了陶瓷过滤器100。两种过程都可以单独或组合进行,从而为过滤器100提供所需的孔径规格。
过程1,在烧结之前,可以通过移除流延膜104的顶层、移除0μm至干燥膜104的最终厚度之间的厚度在干燥之前或之后实现。这可以通过以下方式进行:将溶剂放置在膜104的顶部,使其在那里静置通常长于1秒的时间段,或者将其振荡以加速该过程,之后使用工具400,如流延刀或其他类似的工具将膜104的表面刮擦至洁净,并且之后通过将膜104立刻转移至热烘箱中来蒸发溶剂。膜104暴露于溶剂越长,所制造的孔102越大。另一种过程1中可以使用的方法是使用工具400,如流延刀或其他类似的工具移除膜的顶层(所使用的工具400的间隙越厚,所得到的过滤器100中的孔径越小),或者通过使用柔软工具轻轻地刮擦膜104的表面(取决于强度和/或将此完成期间的时间,将会制造具有可控孔径的膜104)。
可以在除了过程1之外使用或单独使用的过程2在烧结之后进行并且可以获得孔径的更好的可调节控制。这根据时间、压力和所使用的研磨材料(例如“砂纸”或金刚石工具)通过研磨膜104的表面以使得其孔102更大而完成。
使用这个方法,根据所使用的一个或多个过程、在膜104上施加的垂直力、和所使用的一种或多种材料,可以严格控制在膜104的表面的孔径。这有助于包括陶瓷膜盘的底部的一步通用制造过程,其然后在过程1和/或2之后可以针对不同应用进行调节。
如可以从图1中看到的,在横向和2个维度上观察具有锥形几何形状的孔102中,通过改变在较小孔径端的研磨的量,可能产生具有受控、可变尺寸的孔102。
通过这些技术制造的过滤器100可用于膜过滤,其用于血细胞的工业分离以去除白细胞(减小感染风险)。膜过滤是简单且廉价的并且其在该过程期间容易保持无菌。在图6中示出了这样的血液过滤装置600的实例示意图。
如在图6中所示,将过滤器100夹在塑料顶部604和塑料底部610之间。分别在过滤器100与塑料顶部604和塑料底部610之间设置两个密封(O环)606。塑料顶部604包括进料部602,由过滤器100过滤的材料可以通过其***至装置600中。塑料底部610包括开口608,过滤的材料之后可以通过其收集。可以通过金属带将组合件固定在一起。
图7示出了膜过滤器的实施方案的粒子分离的范围。可以看出,可以使用在本文中所描述的技术制造一系列包括具有宽的尺寸范围的孔(在本实例中为~0.1μm至数十μm)的过滤器。将理解的是,可以通过一种或多种待过滤的具体材料的尺寸确定孔的尺寸。
图8示出了使用如在本文中所描述的技术制备的陶瓷过滤器的顶视图。如在示意性横截面图中图示的,切割过滤器以使得切口在接近过滤器的右手边较深。如可以看到的,切口的深度决定了孔的开口尺寸。
图9a示出了过滤器的横截面图。可以看出孔的直径朝向膜过滤器的底部而增加。图9b和c示出了在图9a中图示的过滤器的顶视图。如已经在图8中图示的,由膜的顶部表面的研磨深度决定在过滤器的顶部表面的孔的开口的直径。图9d示出了过滤器的底视图。如上所述,孔的开口直径较大。
图9e示出了在这个实例中具有50mm的直径的膜过滤器的顶部的透视图。如上所述,可以根据过滤器的具体实施来调节膜过滤器的形状。
更通常地,陶瓷过滤器可用于苛刻环境条件(化学/热/pH),以及此外当在分离过程期间或之后需要高压时(例如用于将膜再生)。
当过滤人细胞时,这样的苛刻条件通常不存在,但是通过促进更密集填充的孔结构的形成,陶瓷过滤器的高强度在本申请中提供了重要的优势。这进而有助于通过降低细胞经过过滤器而产生的应力来保持过滤的细胞的形状和活力。
另外的应用
现在描述在本文中所描述的技术的另外的应用:微过滤器是具有在许多不同行业的应用的平台技术。微滤膜可以分离悬浮固体(如金属氢氧化物、微米尺寸粒子、以及宏观物质)、气体(尤其是气泡形式的)、不可混合液体(如在乳状液中)等。被移除的典型物质可以包括细胞、淀粉、细菌、霉菌、酵母、乳化油、灰尘、头发粒子、气泡等。我们在这里提供了另外的应用的非详尽清单,但是一般来说,该技术可用于需要分离具有大于0.1μm的尺寸的粒子的任何应用。通过例如用具有特定性能的一种物质或一组物质涂布无机材料的表面以为过滤器的用途赋予另外的优势,该技术还可以充当另外的产品的起点。
因此,一些实例应用包括:用于研究和开发目的的细胞分离(干细胞等);血液白细胞去除;血液细胞分级;血液回输(bloodsalvage);生物技术/生物制药/制药应用;食品和饮料应用;乳制品应用;涉及饮用水的生成的应用;涉及水的工业加工的应用;废水加工应用;化学和石化应用;在半导体/半导体加工领域中的应用;在电子学与光子学领域中的应用;空气过滤应用;提供反应性孔的结构的应用;气泡的移除;其他物理学和更一般的应用。
这些中的每一个可以采用从流体流中排除落在所描述的技术的尺寸范围内或以上的粒子。通常,微过滤器可以用作用于许多较灵敏的分离的“预过滤器”:例如空气纯化过滤器可能会容易被灰尘和其他粒子堵塞;使用我们描述的技术允许这种较大碎屑的粗分离,延长下游较灵敏的过滤器寿命。现在进行对以上应用中的一些的更详细的描述。
细胞分离
在本文中公开的技术提供基于尺寸差异进行细胞分离的方法。一个实例是,将干细胞和其他祖细胞与完全功能化细胞分离,如将有核网状细胞与无核红细胞分离。
血液白细胞去除
通过收集的全血的白细胞消耗(leukodepletion)或白细胞去除,意指将白细胞从全血或成分如血浆、红细胞或血小板中移除。该技术允许调节过滤器微孔的尺寸以从全部其他较小血细胞/粒子(血浆、血小板和红细胞)中排除血液中存在的较大白细胞。
血液细胞分级
通过使用不同的膜孔径和/或不同的过滤器配置,该***允许将血液分级为其主要组分:血浆、血小板、红细胞和有核细胞。
血液回输
外科手术血液回输是其中使用自动化***收集外科手术期间或之后损失的血液、将其清洁、并且使其可用于向患者再输注的医院操作。在本文中公开的技术可以用作“细胞回收器”装置,其在将血液输注回到患者之前,过滤其以移除污染该血液的任何栓塞物和/或任何大的外部碎屑——尤其是来自外科手术设备的纤维、灰尘或任何其他大粒子。
生物技术/生物制药/制药
该技术具有在其中需要处理较大粒子的应用,例如在抗体或其他来自细胞的活性物质的制备/分离中。该技术也可以用于生物处理、辅助细胞收集、蛋白质浓缩、药物补充水的澄清和制备。其他应用包括精细的进餐和烹饪;最小化加工食品(减少对水/氯的需求)。另外的应用是用于研究的人类***物的分解:这些由有机食品、细菌、蛋白质和小代谢物(例如糖)组成——例如,按照逐渐降低的尺寸,尺寸1可以分离食品碎屑;尺寸2移除细菌;尺寸3移除蛋白质;并且最终尺寸4收集小代谢物。其他应用包括对微胶囊进行尺寸分选;用于体外受精的***活力;在发展中国家的诊断和疾病筛选(例如,可以分离寄生物的卵以检测它们的存在,或者可以移除待分析的液体(水、血液等)以将寄生物浓缩并且因此增加使用普通方法检测的机会);可变和可控尺寸的脂质体(lypossome)(在内部含有分子的结构);利用珠尺寸编码的抗原系细胞分选;探索细胞-细胞信号传导的机制;3D细胞培养物;微胶囊形成(抑制制备期间微胶囊的收缩)。
食品&饮料
这包括在以下领域中的应用:乳制品、酒精饮料(葡萄酒和啤酒)、糖和增甜剂、果汁、蛋白质回收和废水再利用。微滤膜可以用于果汁、葡萄酒、啤酒、醋、糖浆的澄清;葡萄酒和啤酒的冷灭菌;用于乳清过滤;用于牛奶分级和延长牛奶保存期限。该技术还可以用于制造新型牛奶系液体和干燥成分,以及具有高蛋白质含量的低碳水化合物乳制品饮料。这些膜微过滤器还提供在极端食品加工条件下,如污垢、热和化学、以及反复暴露于热水和苛性物质(caustics)的高耐受性,这些是有用的特性。
乳制品
目前,脱脂奶产业使用微滤膜用于其澄清和灭菌。乳制品产业中MF的两个主要应用使用具有1.4或0.1μm平均孔径的膜的过滤器,这目前主要商业用于饮用乳和奶酪用乳。我们的微过滤器可能是更稳健的并且使得能够制造较大孔径的膜,这可以产生较高的流量。
饮用水
该技术可以用于饮用水的生产,尤其是通过直接移除混浊物、寄生物、细菌、囊(cyst)等。此外,其还可以用作对于反渗透和纳米过滤膜分离的预处理。以小增量制造不同的孔径的可能性有助于具有最佳通量/分离性能的过滤膜的具体情况(case-by-casescenario)的形成。在这个范围内的其他应用包括使用反渗透的脱盐设备的预处理:该技术允许从原料进料中移除细菌、胶体粒子、浮游生物和藻类,这可以增加较昂贵的反渗透膜的寿命。
工业过程水
受益于这种技术的优势的产业包括大量水用户,如发电厂、油气生产商、和化学制造商。例如,在花粉、灰尘、昆虫、废气等中冷却塔捕获接近3kg/天,同时在用于再循环的水收集区域随时间发现了生物膜的形成(build-up),这降低并且甚至完全阻塞了回收***。这些并非必须为“可饮用质量”的水的预处理可以有助于降低运行这些行业的成本。其他应用包括在反渗透和纳米过滤膜过滤前的预处理。该技术还可以用于分离和/或回收催化剂、苛性物质、脱脂剂、染料、上浆剂、油/水乳液的分离等等。
废水
在本文中公开的技术可以移除细菌、贾第鞭毛虫(Giardia)和其他来自受污染的水的微生物,并且例如从工业过程移除重金属用于回收。由于它们特定的强度,我们描述的膜还可以用于放射性废物的清理,用于处理核洗涤废水和从水流中移除铀。它们可以用于分离和/或回收催化剂、苛性物质、脱脂剂、染料、上浆剂、油/水乳液的分离等等。该技术还可以用作对借助反渗透、纳米过滤或超滤膜分离的其他下游过滤方法的预处理:不含大粒子和污染物的废水将会增加寿命并且因此导致较昂贵的反渗透膜、纳米过滤膜和超滤膜的成本降低。
化学&石化产业
公开的微滤膜可以用作超纯水制造方法的一部分并且用于化学废水的解毒,尤其是作为预处理屏障。可以在化学产业中使用过滤器用于二级和三级催化剂回收、溶剂回收、化学澄清,和用于从进入反应器过程的进料物流中移除固体和液体污染物。在这些领域中的其他用途包括作为用于化学溶液沉积的过滤器(在薄膜技术中),以从石油和天然气开采中移除大粒子(如灰尘),以及用于其他下游的精炼过程。
电子学/光子学/半导体
如在化学纯化和铜浆料过滤中的应用可以使用所公开的技术。所公开的技术还可以用作用于如光刻压印(lithographyimprinting)的应用的罩。孔可以起光导的作用,并且在漏斗的窄端可以有效地减小斑点尺寸,因此可以增加光导准确性并且降低散射。使光照射通过根据预定结构排列的、具有不同孔径的膜孔还可以用于相关应用,例如,将预定形状形成到置于膜的另一侧的物体上。该技术还可以用于粒子/光轨迹的排列。可以使用该结构的又一个大规模实施方案,例如作为宣传或显示面板,例如通过将图像图案化至过滤器中,其之后可以用于投射光和/或类似于窗口观察。这也可以使用“秘密通信”——过滤器可以带有仅在将光照射通过过滤器时可见的图像。
空气
该技术可以用于非液体介质,尤其是用于纯化或处理空气或其他气体。例如,该技术可以用作借助纳米过滤或超滤膜分离的其他空气过滤方法的预处理(通常用于移除气味或空气携带的病毒)。移除空气携带的大粒子如灰尘、头发粒子等可以增加较昂贵的纳米过滤膜和超滤膜的寿命。在空气过滤中的许多其他应用也是可能的。
反应孔
如果仅研磨膜的一侧,所得到的孔可以用于多个应用,如用于间歇式化学反应。
物理学
应用不限于过滤物理粒子。该技术可以用于光学衍射光栅;表面等离激元;超材料(metamaterial)波导(其使用均匀隔开的孔);不常见几何形状过滤器;与称重传感器偶联(以允许例如量化通过的物质的量);用于测试粒子的球度;作为用于高纯度粉末和纳米粉末的筛;X射线衍射;用于空气动力学(通过构建具有由孔得到的特殊空气动力学特征的结构);利用孔结构形成石墨烯;用于3D的电脑的有机开关;作为用于光谱法的粒径过滤器(以过滤为<100μm从而抑制光散射);作为控制材料生长的硬质罩(操作材料加工);用于制造图案化纳米材料;等等。
气泡的移除
微米尺寸的气泡,如空气气泡在某些产业中是有害的。实例包括其中使用注塑成型或将熔融金属倾倒至模具中以制造汽车轮毂、窗口把手的产业。通常,在用于制造采用将介质熔融并且将其倾倒至模具中接着凝固(例如,通过温度降低,与非溶剂接触,蒸发,或其他技术)的制造步骤的产品的过程中,空气气泡和/或未溶解粒子的存在可能会导致问题。尤其是,空气气泡或未溶解粒子的存在可能会损害这样的产品的结构,可能导致断裂和损坏。在介质过滤前,任选在升高的温温度,可以使用在本文中公开的技术移除空气气泡(其可以是微米尺寸的)或未溶解粒子(其可以是较大的)。
其他应用
在本文中公开的技术还可以用于许多其他领域,例如:空气测试/汽车碎屑过滤器;油分离(尤其是来自泥土碎屑和其他大粒子);家用用途(在真空吸尘器等中);在燃气灶中以更有效地燃烧气体;作为过敏原过滤器,例如用于哮喘;以提供用于空调的花粉过滤器和其他类似应用;作为用于例如汽车应用的自清洁过滤器(取决于陶瓷盘坚固性(ruggedness)和不堵塞性质);在农业中,例如用于分选种子;等等。
该技术还可以用作后处理的起点以使该技术适用于之前描述的或其他应用。尤其是,可以通过方法如等离子体处理、化学蚀刻或交联、吸附或任何其他涂布方法修饰过滤器的表面。这是尤其可用的,从而向过滤器膜添加下列各项中的一种或多种:功能化生物分子如氨基酸;抗微生物化合物如铜、银、金或任何其他金属或这些的混合物;氧化剂如氧化硼(III)、氧化硅(IV)、氧化铬(III)、氧化锰(IV)、氧化铁(III)、氧化铁(II,III)、氧化铜(II)、氧化铅(II、IV)等等;以及可以使得膜过滤器更少或更多透过特定或一组粒子或物质的其他化学元素或分子(例如,基于电荷、分子量、尺寸、迁移率、化学亲和力等等,例如用于目标细胞类型或者目标分子)。
毫无疑问,对于技术人员来说,将存在许多其他有效的替代方案。应理解的是,本发明不限于所描述的实施方案并且包括在所附权利要求的精神和范围内的对于对本领域技术人员来说显而易见的改进。
Claims (21)
1.一种制造具有受控过滤器通道开口尺寸的陶瓷过滤器的方法,所述方法包括:
制造陶瓷前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含陶瓷材料;以及
烧结所述陶瓷前体元件以使所述陶瓷材料融合并且移除所述聚合物材料;
所述方法还包括移除所述第一表面的受控厚度部分以使所述呈喇叭形展开的孔开口至所述受控过滤器通道开口尺寸。
2.根据权利要求1所述的方法,其中所述受控厚度部分的所述移除包括将溶剂沉积至所述陶瓷前体元件的所述第一表面上。
3.根据权利要求1或2所述的方法,其中所述受控厚度部分的所述移除包括从所述陶瓷前体元件的所述第一表面物理移除受控的厚度。
4.根据权利要求1、2或3所述的方法,其中所述受控厚度部分的所述移除包括研磨所述烧结的陶瓷前体元件的所述第一表面。
5.根据任一项前述权利要求所述的方法,其中所述陶瓷前体元件的所述制造包括:
将包含所述陶瓷材料、所述聚合物、和用于所述聚合物的溶剂的掺杂剂形成为用于所述陶瓷前体元件的形状;和
在其中所述溶剂可溶混的液体浴中处理所述形成的形状。
6.根据权利要求5所述的方法,其中所述陶瓷前体元件的所述形状是片状或管状。
7.根据任一项前述权利要求所述的方法,所述方法还包括移除所述第二表面的一部分以使所述呈喇叭形展开的孔开口。
8.根据任一项前述权利要求所述的方法,所述方法还包括在制造之后向所述过滤器应用表面改性处理以改变所述过滤器的过滤特性。
9.一种使用任一项前述权利要求所述的陶瓷过滤器过滤细胞、尤其是血细胞的方法。
10.一种陶瓷过滤器,所述陶瓷过滤器由根据权利要求1至8中任一项所述的方法制造。
11.一种陶瓷过滤器,所述陶瓷过滤器具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸以及与所述第一和第二表面连接的呈喇叭形展开的通道的排列。
12.根据权利要求11所述的陶瓷过滤器,其中所述呈喇叭形展开的通道的开口通常是圆形的并且多于90%具有大于0.1μm的直径。
13.根据权利要求12所述的陶瓷过滤器,其中所述呈喇叭形展开的通道的所述开口的多于90%具有小于50μm、优选小于5μm的直径。
14.根据权利要求9至14中任一项所述的陶瓷过滤器,其中所述过滤器的表面具有功能化的表面涂层或处理。
15.血液过滤装置,所述血液过滤装置包括根据权利要求9至14中任一项所述的过滤器。
16.一种制造无机过滤器的方法,所述方法包括:
制造前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含无机材料;以及
烧结所述前体元件以使所述无机材料融合并且移除所述聚合物材料;
所述方法还包括移除所述第一表面的一部分以使所述呈喇叭形展开的孔开口。
17.一种陶瓷过滤器,所述陶瓷过滤器由根据权利要求16所述的方法制造。
18.一种使用根据权利要求9至14和17中任一项所述的过滤器从流体中过滤粒子的方法。
19.一种制造罩的方法,所述方法包括:
制造陶瓷前体元件,所述前体元件具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸的呈喇叭形展开的孔的排列,其中所述呈喇叭形展开的孔的顶点朝向所述第一表面并且所述呈喇叭形展开的孔的底部朝向所述第二表面并且大于所述顶点,其中所述呈喇叭形展开的孔含有聚合物材料并且所述呈喇叭形展开的孔之间的区域包含陶瓷材料;以及
烧结所述陶瓷前体元件以使所述陶瓷材料融合并且移除所述聚合物材料;
所述方法还包括移除所述第一表面的受控厚度部分以使所述呈喇叭形展开的孔开口至所述受控通道开口尺寸。
20.根据权利要求19所述的方法,所述方法还包括将在所述第一和第二表面之一或二者上的孔开口图案化。
21.一种罩,尤其是由根据权利要求19或20所述的方法制造的罩,所述罩具有包括第一和第二表面的结构以及在所述第一和第二表面之间延伸并且与所述第一和第二表面连接的呈喇叭形展开的通道的排列,以提供通过所述罩的呈喇叭形展开的、透光通道,其中将所述板/罩结构的所述呈喇叭形展开的通道的排列图案化以限定用于所述罩的透光图案。
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