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CN104083930B - A kind of filtrating chip and processing and fabricating method thereof - Google Patents

A kind of filtrating chip and processing and fabricating method thereof Download PDF

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CN104083930B
CN104083930B CN201410318034.5A CN201410318034A CN104083930B CN 104083930 B CN104083930 B CN 104083930B CN 201410318034 A CN201410318034 A CN 201410318034A CN 104083930 B CN104083930 B CN 104083930B
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filter structure
substrate
chip
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micro
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CN104083930A (en
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黄伟
李丰
杨立梅
张巍巍
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Abstract

本发明涉及一种过滤芯片,同时还涉及过滤芯片的制作方法,属于环境、食品、化工和医药等领域。该芯片包括具有过滤结构的衬底、上盖、正向进样口、正向出样口、反向回冲进样口、反向回冲出样口,芯片一侧由近及远依次排列着分别与过滤结构相连通的反向回冲出样口、正向进样口,芯片另一侧由近及远依次排列着分别与过滤结构相连通的正向出样口、反向回冲进样口,所述过滤结构由一系列具有间隙呈柱状阵列的微纳柱体组成的,分为内过滤结构和外过滤结构,具有过滤结构的衬底和上盖通过衬底上的分布于内过滤结构内部的固定柱和外过滤结构外部的固定柱绑定在一起。本发明回收率高、可承受高流速、成本低、适于大规模量产,可广泛用于水、食品及微生物领域微颗粒的过滤和浓缩。

The invention relates to a filter chip and a manufacturing method of the filter chip, belonging to the fields of environment, food, chemical industry, medicine and the like. The chip includes a substrate with a filter structure, an upper cover, a forward sample inlet, a forward sample outlet, a reverse backflush inlet, and a reverse backflush outlet. One side of the chip is arranged in order from near to far. Next to the reverse backflush sample port and forward sample inlet connected to the filter structure, the other side of the chip is arranged in sequence from near to far with the forward sample outlet and reverse backflush respectively connected to the filter structure. Inlet, the filter structure is composed of a series of micro-nano cylinders with gaps in a columnar array, divided into inner filter structure and outer filter structure, the substrate with filter structure and the upper cover are distributed on the substrate The fixed columns inside the inner filter structure are bound together with the fixed columns outside the outer filter structure. The invention has high recovery rate, can withstand high flow rate, low cost, is suitable for large-scale mass production, and can be widely used in the filtration and concentration of microparticles in the fields of water, food and microorganisms.

Description

一种过滤芯片及其加工制作方法A filter chip and its manufacturing method

技术领域technical field

本发明涉及一种过滤芯片及其加工制作方法,属于环境、食品、化工和医药等领域。The invention relates to a filter chip and a processing and manufacturing method thereof, belonging to the fields of environment, food, chemical industry, medicine and the like.

背景技术Background technique

微纳过滤器作为常见的过滤膜,广泛应用于饮用水中微生物分析、葡萄酒和果汁的无菌过滤及无菌药物筛选等领域。按照工作模式,微纳过滤器可分为死端过滤和错流过滤。死端过滤是将待过滤样置于过滤器正上方,在压力差的推动下,大于过滤器典型孔径尺寸的颗粒被截留在膜上。这种过滤器随着时间推移,颗粒易在膜表面形成堵塞,使得过滤阻力增加。错流过滤模式在膜表面产生两种分力,垂直于流向的法向力使得样品通过过滤间隙,沿着流向的切向力使得截留颗粒物较均匀散开,这种过滤膜不易产生浓度极化和结垢问题。当前微纳过滤器的主要制作方法包括硅面型微加工方法、相分离微成型方法和孔径阵列光刻方法。这些方法的问题和不足在于:脱模时存在塌陷或破损等问题,过滤器强度低、成本高、产率低。As a common filtration membrane, micro-nano filters are widely used in the fields of microbial analysis in drinking water, sterile filtration of wine and fruit juice, and sterile drug screening. According to the working mode, micro-nano filters can be divided into dead-end filtration and cross-flow filtration. Dead-end filtration is to place the sample to be filtered directly above the filter, and driven by the pressure difference, particles larger than the typical pore size of the filter are trapped on the membrane. With the passage of time, the filter is easy to be blocked by particles on the surface of the membrane, which increases the filtration resistance. The cross-flow filtration mode produces two component forces on the surface of the membrane. The normal force perpendicular to the flow direction makes the sample pass through the filter gap, and the tangential force along the flow direction makes the trapped particles more evenly scattered. This kind of filter membrane is not easy to produce concentration polarization. and fouling problems. The current main fabrication methods of micro-nano filters include silicon surface micromachining method, phase separation micromolding method and aperture array photolithography method. The problems and deficiencies of these methods are: there are problems such as collapse or damage during demoulding, and the filter has low strength, high cost and low yield.

微纳过滤器的一种典型应用是用于水中颗粒物的过滤浓缩,如水源性寄生虫卵隐孢子虫和贾第鞭毛虫。目前,饮用水中隐孢子寄生虫和贾第鞭毛寄生虫标准检测方法为美国国家环境保护局(USEPA)制定的EPA 1623方法。EPA 1623方法主要包括过滤和洗提、浓缩和分离、免疫荧光标记和荧光显微镜分析等步骤。该方法技术成熟、认可度高,但也有其局限性:耗时3-7天、成本高、步骤繁琐,且易受水中藻类的交叉反应影响,回收率不高。EPA 1623方法所用高分子过滤器由于制作工艺的限制,无法承受高流速,无法对于所截留得微生物进行自动回收,必须手动振荡并洗脱,回收率低、成本高。A typical application of micro-nano filters is for the filtration and concentration of particulate matter in water, such as the eggs of water-borne parasites Cryptosporidium and Giardia. Currently, the standard detection method for cryptosporidium parasites and giardia parasites in drinking water is the EPA 1623 method formulated by the US Environmental Protection Agency (USEPA). The EPA 1623 method mainly includes steps such as filtration and elution, concentration and separation, immunofluorescence labeling, and fluorescence microscopy analysis. This method is mature and highly recognized, but it also has its limitations: it takes 3-7 days, high cost, cumbersome steps, and is easily affected by cross-reaction of algae in water, and the recovery rate is not high. Due to the limitations of the manufacturing process, the polymer filter used in the EPA 1623 method cannot withstand high flow rates and cannot automatically recover the trapped microorganisms. It must be manually oscillated and eluted, resulting in low recovery and high cost.

发明内容Contents of the invention

本发明的目的在于:针对上述现有技术存在的弊端,提出一种过滤芯片,同时还给出过滤芯片的制作方法。The object of the present invention is to propose a filter chip and a method for making the filter chip in view of the disadvantages of the above-mentioned prior art.

为了达到以上目的,本发明采取的技术方案是使得过滤芯片包括具有过滤结构的衬底、上盖、正向进样口、正向出样口、反向回冲进样口、反向回冲出样口,芯片一侧由近及远依次排列着分别与过滤结构相连通的反向回冲出样口、正向进样口,芯片另一侧由近及远依次排列着分别与过滤结构相连通的正向出样口、反所述过滤结构由一系列具有间隙呈柱状阵列的微纳柱体组成的,分为内过滤结构和外过滤结构,具有过滤结构的衬底和上盖通过衬底上未刻蚀部分的固定柱牢固绑定在一起。In order to achieve the above purpose, the technical solution adopted by the present invention is to make the filter chip include a substrate with a filter structure, an upper cover, a forward sample inlet, a forward sample outlet, a reverse backflush inlet, a reverse backflush The sample outlet, one side of the chip is arranged in sequence from near to far with reverse backflush outlet and forward inlet which are respectively connected to the filter structure, and on the other side of the chip are arranged in turn from near to far respectively connected to the filter structure. The connected positive sample outlet and reverse filter structure are composed of a series of micro-nano cylinders with gaps in a columnar array, which are divided into inner filter structure and outer filter structure. The substrate with filter structure and the upper cover pass through The anchor posts on the unetched part of the substrate are firmly bound together.

具体地说内过滤结构和外过滤结构的间隙为非均匀设计;所述微纳柱体可为方形、圆柱形、梯形形状、类雨滴形状,或其他各种类似形状;Specifically, the gap between the inner filter structure and the outer filter structure is non-uniform design; the micro-nano column can be square, cylindrical, trapezoidal, raindrop-like, or other similar shapes;

进一步地,内过滤结构和外过滤结构间隙的大小呈错开排列;所述衬底是硅或玻璃。Further, the size of the gap between the inner filter structure and the outer filter structure is staggered; the substrate is silicon or glass.

本发明的过滤芯片的制作方法,包括以下步骤:The manufacturing method of filter chip of the present invention comprises the following steps:

第一步、先制作出具有单分子防粘层的有微纳间隙的软模板;The first step is to make a soft template with micro-nano gaps with a monomolecular anti-sticking layer;

第二步、在衬底上旋涂过渡胶层然后再涂上压印光刻胶层,制成基片;The second step is to spin-coat the transition glue layer on the substrate and then coat the embossed photoresist layer to make the substrate;

第三步、将软模板和基片上的压印光刻胶层对准,将软模板上图案转移到压印胶上,形成由压印光刻胶构成的微纳柱;The third step is to align the soft template with the embossed photoresist layer on the substrate, transfer the pattern on the soft template to the imprinted glue, and form micro-nano pillars composed of the imprinted photoresist;

第四步、采用反应离子刻蚀工艺依次去除微纳柱之间的压印光刻胶层残余及微纳柱之间的压印光刻胶层残余下面的过渡层,露出衬底;The fourth step is to sequentially remove the residual imprinted photoresist layer between the micro-nano pillars and the transition layer under the residual imprinted photoresist layer between the micro-nano pillars by using a reactive ion etching process to expose the substrate;

第五步、采用电子束蒸发工艺在样品表面蒸镀金属薄层,并利用丙酮溶液清洗基底表面的过渡胶层及其上的压印胶层和金属薄层从而剩下衬底表面的金属薄层作为掩膜层;The fifth step is to evaporate a thin metal layer on the surface of the sample by electron beam evaporation, and use acetone solution to clean the transition adhesive layer on the surface of the substrate and the embossed adhesive layer and thin metal layer on it to leave the thin metal layer on the substrate surface. layer as a mask layer;

第六步、利用金属薄层作为掩膜,采用电感耦合等离子体刻蚀工艺刻蚀衬底,而后采用清洗液祛除掩膜层,在衬底上获得对应的图案和结构。Step 6: Using the thin metal layer as a mask, the substrate is etched by an inductively coupled plasma etching process, and then the mask layer is removed with a cleaning solution to obtain a corresponding pattern and structure on the substrate.

进一步地所述的过滤芯片的制作方法,所述金属薄层所用金属是镍。Further, in the manufacturing method of the filter chip, the metal used in the thin metal layer is nickel.

本发明的有益效果是:这种微纳过滤芯片回收率高、可承受高流速、成本低、适于大规模量产,可广泛用于水、食品及微生物领域微颗粒的过滤和浓缩。The beneficial effects of the invention are: the micro-nano filtration chip has high recovery rate, can withstand high flow rate, low cost, is suitable for large-scale mass production, and can be widely used in the filtration and concentration of micro-particles in the fields of water, food and microorganisms.

附图说明:Description of drawings:

下面结合附图对本发明作进一步说明。The present invention will be further described below in conjunction with accompanying drawing.

图1是本发明的结构示意图一;Fig. 1 is a structural schematic diagram one of the present invention;

图2是本发明的结构示意图二;Fig. 2 is a structural schematic diagram two of the present invention;

图3是过滤微结构截面图一;Fig. 3 is a cross-sectional view of the filtering microstructure;

图4是过滤微结构截面图二;Fig. 4 is the second cross-sectional view of the filtering microstructure;

图5是过滤微结构截面图三;Fig. 5 is the third cross-sectional view of the filtering microstructure;

图6是过滤微结构截面图四;Figure 6 is a cross-sectional view of the filter microstructure four;

图7是压印制作工艺示意图;Fig. 7 is a schematic diagram of the embossing manufacturing process;

具体实施方式Detailed ways

下面结合具体实施方式对本发明做进一步详细叙述。The present invention will be further described in detail below in combination with specific embodiments.

本实施例的过滤芯片装置如图1-6所示,包括具有过滤结构5和9的硅制成的衬底15、玻璃上盖16、正向进样口1、正向出样口3、反向回冲进样口4、反向回冲出样口2,芯片一侧由近及远依次排列着分别与过滤结构相连通的反向回冲出样口2、正向进样口1,芯片另一侧由近及远依次排列着分别与过滤结构相连通的正向出样口3、反向回冲进样口4,所述过滤结构5和9由一系列阵列排列的微纳柱体17组成的,分为内过滤结构5和外过滤结构9,具有过滤结构的衬底和上盖通过衬底上的分布于内过滤结构内部的固定柱13和外过滤结构外部的固定柱14绑定在一起。13和14为芯片中未刻蚀区域,为流样提供导引,同时增大绑定接触面积,提高芯片抗压性能。芯片工作时,待过滤浓缩大体积样从1进入,过滤后洁净水样从3流出。过滤时,流样中处于内过滤结构6(间隙大于粒子直径)附近的粒子可从此处大间隙离开,并被外围过滤结构10(间隙小于粒子直径)所俘获。处于内过滤结构7的粒子直接被俘获(间隙小于粒子直径)。其他位置处粒子俘获原理依次类推。粒子被俘获后,用少量的去离子水从4反向回冲芯片,所俘获的粒子即被释放,实现过滤浓缩目的。The filter chip device of the present embodiment is as shown in Figure 1-6, comprises the substrate 15 that the silicon that has filtering structure 5 and 9 is made, glass upper cover 16, forward sample inlet 1, forward sample outlet 3, Reverse backflush inlet 4, reverse backflush outlet 2, reverse backflush outlet 2, forward inlet 1 respectively connected to the filter structure are arranged in order from near to far on the chip side On the other side of the chip, forward sample outlet 3 and reverse backflush inlet 4 respectively connected to the filter structure are arranged in order from near to far. The filter structures 5 and 9 are composed of a series of micro-nano Composed of cylinders 17, it is divided into an inner filter structure 5 and an outer filter structure 9. The substrate with the filter structure and the upper cover pass through the fixed columns 13 distributed inside the inner filter structure and the fixed columns outside the outer filter structure on the substrate. 14 bound together. 13 and 14 are unetched areas in the chip, which provide guidance for flow samples, increase the bonding contact area, and improve the pressure resistance of the chip. When the chip is working, the large-volume sample to be filtered and concentrated enters from 1, and the filtered clean water sample flows out from 3. When filtering, the particles in the flow sample near the inner filter structure 6 (the gap is larger than the particle diameter) can leave the large gap here and be captured by the peripheral filter structure 10 (the gap is smaller than the particle diameter). Particles in the inner filter structure 7 are directly trapped (gap smaller than particle diameter). The principle of particle capture at other positions can be deduced by analogy. After the particles are captured, use a small amount of deionized water to reversely flush the chip from 4, and the captured particles are released to achieve the purpose of filtration and concentration.

具体地说内过滤结构5和外过滤结构9的间隙为非均匀设计;所述微纳柱体17可为方形、圆柱形、梯形形状、类雨滴形状,或其他各种类似形状;Specifically, the gap between the inner filter structure 5 and the outer filter structure 9 is non-uniform; the micro-nano column 17 can be square, cylindrical, trapezoidal, raindrop-like, or other similar shapes;

进一步地,内过滤结构5和外过滤结构9中微纳柱体17间间隙的大小呈错开排列;如内过滤层的6为大间隙,外过滤层的10为小间隙;内过滤层的7为小间隙,外过滤层的11为大间隙;内过滤层的8为大间隙,外过滤层的12为小间隙。Further, the size of the gap between the micro-nano cylinders 17 in the inner filter structure 5 and the outer filter structure 9 is staggered; as 6 of the inner filter layer is a large gap, 10 of the outer filter layer is a small gap; 7 of the inner filter layer 11 of the outer filter layer is a large gap; 8 of the inner filter layer is a large gap, and 12 of the outer filter layer is a small gap.

如图7所示,制作过滤芯片按以下步骤进行:As shown in Figure 7, making the filter chip is carried out according to the following steps:

第一步、先制作出表面具有单分子防粘层的有弹性支撑层、硬质结构层、有微纳间隙图案的软模板23;The first step is to make an elastic support layer with a monomolecular anti-adhesive layer on the surface, a hard structure layer, and a soft template 23 with micro-nano gap patterns;

第二步、在硅衬底15上旋涂过渡胶层PMMA层22然后再涂上压印光刻胶层UV层21,制成基片;Second step, on the silicon substrate 15, spin-coat the transition glue layer PMMA layer 22 and then coat the embossed photoresist layer UV layer 21 to make the substrate;

第三步、将软模板和基片的UV层对准将软模板上图案转移到压印胶上,形成由压印光刻胶构成的微纳柱;The third step is to align the UV layer of the soft template and the substrate and transfer the pattern on the soft template to the embossing glue to form micro-nano pillars composed of embossing photoresist;

第四步、采用反应离子刻蚀工艺依次去除微纳柱之间的UV层残余及微纳柱之间的UV层残余下面的PMMA层,露出衬底;The fourth step is to sequentially remove the UV layer residue between the micro-nano pillars and the PMMA layer under the UV layer residue between the micro-nano pillars by using a reactive ion etching process to expose the substrate;

第五步、采用电子束蒸发工艺在样品表面蒸镀金属镍25,并利用丙酮溶液清洗基底表面的UV层及其上的压印胶和金属镍,从而剩下衬底表面的金属镍作为掩膜层;The fifth step is to vapor-deposit metal nickel 25 on the surface of the sample by electron beam evaporation process, and use acetone solution to clean the UV layer on the surface of the substrate and the imprinting glue and metal nickel on it, so that the metal nickel on the surface of the substrate is left as a mask. film layer;

第六步、利用金属镍作为掩膜,采用电感耦合等离子体刻蚀工艺刻蚀衬底,而后采用清洗液祛除掩膜层,在衬底上获得对应的图案和结构。The sixth step is to use metal nickel as a mask to etch the substrate by an inductively coupled plasma etching process, and then use a cleaning solution to remove the mask layer to obtain a corresponding pattern and structure on the substrate.

本发明不局限于上述实施例,凡采用等同替换形成的技术方案,均落在本发明要求的保护范围内。The present invention is not limited to the above-mentioned embodiments, and all technical solutions formed by equivalent replacements fall within the scope of protection required by the present invention.

Claims (5)

1.一种过滤芯片,其特征是:所述芯片包括具有过滤结构的衬底、上盖、正向进样口、正向出样口、反向回冲进样口、反向回冲出样口,芯片一侧由近及远依次排列着分别与过滤结构相连通的反向回冲出样口、正向进样口,芯片另一侧由近及远依次排列着分别与过滤结构相连通的正向出样口、反向回冲进样口,所述过滤结构由一系列具有间隙呈柱状阵列的微纳柱体组成的,分为内过滤结构和外过滤结构,具有过滤结构的衬底和上盖通过衬底上的分布于内过滤结构内部的固定柱和外过滤结构外部的固定柱绑定在一起;内过滤结构和外过滤结构的间隙为非均匀设计,且内过滤结构和外过滤结构间隙的大小呈错开排列。1. A filter chip, characterized in that: the chip includes a substrate with a filter structure, an upper cover, a forward sample inlet, a forward sample outlet, a reverse backflush sample inlet, a reverse backflush out The sample port, one side of the chip is arranged in sequence from near to far, the reverse backflush sample port and the forward sample port are respectively connected to the filter structure, and the other side of the chip is arranged in sequence from near to far, respectively connected to the filter structure The forward sample outlet and the reverse backflush inlet are connected. The filter structure is composed of a series of micro-nano cylinders with gaps in a columnar array, which are divided into an inner filter structure and an outer filter structure. The substrate and the upper cover are bound together through the fixed columns distributed inside the inner filter structure on the substrate and the fixed columns outside the outer filter structure; the gap between the inner filter structure and the outer filter structure is non-uniform design, and the inner filter structure The size of the gap with the outer filter structure is arranged in a staggered manner. 2.如权利要求1所述的一种过滤芯片,其特征是:所述微纳柱体为方形或圆柱形或梯形形状或类雨滴形状。2. A filter chip according to claim 1, characterized in that: the micro-nano cylinders are square, cylindrical, trapezoidal or raindrop-like. 3.如权利要求1所述的一种过滤芯片,其特征是:所述衬底是硅或玻璃。3. A filter chip as claimed in claim 1, characterized in that: said substrate is silicon or glass. 4.一种如权利要求1所述的过滤芯片的加工制作方法,其特征是包括以下步骤:4. A method for processing a filter chip as claimed in claim 1, characterized in that it comprises the following steps: 第一步、先制作出具有单分子防粘层的有微纳间隙的软模板;The first step is to make a soft template with micro-nano gaps with a monomolecular anti-sticking layer; 第二步、在衬底上旋涂过渡胶层然后再涂上压印光刻胶层;The second step is to spin-coat the transition layer on the substrate and then apply the imprint photoresist layer; 第三步、将软模板和衬底上的压印光刻胶层对准,将软模板上图案转移到压印胶上,形成由压印光刻胶构成的微纳柱;The third step is to align the soft template with the embossed photoresist layer on the substrate, transfer the pattern on the soft template to the imprinted glue, and form micro-nano pillars composed of the imprinted photoresist; 第四步、采用反应离子刻蚀工艺依次去除微纳柱之间的压印光刻胶层残余及微纳柱之间的压印光刻胶层残余下面的过渡层,露出衬底;The fourth step is to sequentially remove the residual imprinted photoresist layer between the micro-nano pillars and the transition layer under the residual imprinted photoresist layer between the micro-nano pillars by using a reactive ion etching process to expose the substrate; 第五步、采用电子束蒸发工艺在样品表面蒸镀金属薄层,并利用丙酮溶液清洗基底表面的过渡胶层及其上的压印光刻胶层和金属薄层从而剩下衬底表面的金属薄层作为掩膜层;The fifth step is to evaporate a thin metal layer on the surface of the sample by electron beam evaporation, and use acetone solution to clean the transition layer on the surface of the substrate and the imprinted photoresist layer and thin metal layer on the surface of the substrate to leave the surface of the substrate. A thin metal layer as a mask layer; 第六步、利用金属薄层作为掩膜,采用电感耦合等离子体刻蚀工艺刻蚀衬底,而后采用清洗液祛除掩膜层,在衬底上获得对应的图案和结构。Step 6: Using the thin metal layer as a mask, the substrate is etched by an inductively coupled plasma etching process, and then the mask layer is removed with a cleaning solution to obtain a corresponding pattern and structure on the substrate. 5.如权利要求4所述的一种过滤芯片的加工制作方法,其特征是:所述金属薄层所用金属是镍。5. The manufacturing method of a filter chip as claimed in claim 4, wherein the metal used in the thin metal layer is nickel.
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