WO2021000851A1 - 制备图案化聚合物的方法 - Google Patents
制备图案化聚合物的方法 Download PDFInfo
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- WO2021000851A1 WO2021000851A1 PCT/CN2020/099216 CN2020099216W WO2021000851A1 WO 2021000851 A1 WO2021000851 A1 WO 2021000851A1 CN 2020099216 W CN2020099216 W CN 2020099216W WO 2021000851 A1 WO2021000851 A1 WO 2021000851A1
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0035—Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
Definitions
- This application relates to the technical field of microfluidic chips, in particular to a method for preparing patterned polymers.
- Microfluidic chip technology integrates basic operation units such as sample preparation, reaction, separation, and detection in biological, chemical, and medical analysis processes onto a micron-scale chip to automatically complete the entire analysis process. Due to its great potential in the fields of biology, chemistry, medicine, etc., it has developed into a new research field that intersects disciplines such as biology, chemistry, medicine, fluids, electronics, materials, and machinery.
- microfluidic chips can be processed using materials such as glass, polymers, hydrogels, and paper, but the most common materials are polymers.
- silicones such as polydimethylsiloxane (PDMS) are widely used in polymers, and other types of polymers such as polymethyl methacrylate and polycarbonate also have certain applications.
- PDMS polydimethylsiloxane
- the polymer has stable properties, especially the low surface energy of organic silica gel, so it is difficult to achieve high-quality direct photolithography patterning processing, and the use of a large amount of organic solvents such as toluene in the process is extremely harmful to the environment.
- the current process mostly uses the indirect pattern processing method of the inverted mold. The method first uses a standard photolithography method to transfer the pattern to a photoresist such as SU-8 through a mask to prepare a mold with thickness and pattern. Then, the polymer is poured on the surface of the mold made of photoresist, and then peeled off from the mold after drying to obtain a patterned polymer.
- the patterned polymer needs to be carefully peeled off from the photoresist mold.
- the main purpose of this application is to provide a method for preparing patterned polymers with simple process flow and stable production quality.
- a method for preparing a patterned polymer characterized in that it comprises the following steps:
- Spraying photoresist coating a layer of base photoresist on the surface of the base material
- Pattern transfer make a patterned optical reticle, place the optical reticle above the base photoresist and irradiate the pattern on the optical reticle with ultraviolet light to transfer to the base photoresist;
- the base photoresist is developed using a developer whose main component is sodium carbonate to obtain a patterned photoresist on the base material;
- Coating polymer drying the base material and patterned photoresist, coat a polymer layer with a thickness less than that of the patterned photoresist on the surface of the base material, and let it stand until the polymer layer is fully leveled;
- Dissolving polymer heating and baking the polymer layer until it is fully crosslinked and solidified, and then treating the polymer layer with an organic solvent, strong acid or strong base to slowly dissolve the polymer on the top surface of the patterned photoresist;
- Photoresist demolding the patterned photoresist and polymer layer are treated with a stripping solution whose main component is strong alkali, followed by washing and ultrasonic treatment to obtain a patterned polymer.
- step S2 when ultraviolet light irradiates the photomask placed on the base photoresist, the exposed area of the base photoresist is cross-linked and cured to become a non-water-soluble patterned photoresist.
- step S3 it is left during development, and the rest is washed away, completing the first pattern transfer.
- step S4 coat a polymer layer on the surface of the base material and make the thickness of the polymer layer smaller than the thickness of the patterned photoresist, and then in step S5, after the polymer is leveled and cured, it is treated with an organic solvent, a strong acid or a strong base , The thinner polymer layer on the top surface of the patterned photoresist is slowly dissolved; finally, in step S6, the patterned photoresist is gradually cracked and dispersed by the release liquid, and finally peeled off from the base material to realize the second pattern Transfer and obtain a patterned polymer at the same time.
- the method of separating the polymer from the patterned photoresist is to dissolve the patterned photoresist through the release liquid, so that the patterned photoresist is gradually cracked and dispersed into small particles and separated from the polymer , Thereby obtaining a patterned polymer.
- the separation between polymer and patterned photoresist is converted from traditional peeling to dissolution separation.
- the separation process between polymer and patterned photoresist is more gentle, the patterned polymer structure is not easily damaged, and the production quality is higher. Moreover, the operation difficulty, equipment accuracy, and operating environment requirements are lower, the production quality is more stable, and the production is more efficient.
- the ultraviolet light wavelength ⁇ ranges from 315 to 400 nm, and the light intensity i is from 0.1 to 100 mW/cm 2 .
- the base photoresist undergoes crosslinking and curing after being irradiated by ultraviolet light to form an insoluble network structure.
- the mechanism is: polyvinyl alcohol laurate and other materials
- the produced photoresist (photosensitive material) is opened under the action of light, and the double bonds in the molecules are opened, and the chains are cross-linked and then cured to form an insoluble network structure.
- the opening of the double bond requires energy to be absorbed, which is the bond energy.
- the light energy is related to the wavelength of light and the intensity of the light. Therefore, only the ultraviolet light within this wavelength range and light intensity can be absorbed by the double bond to open the double bond. Realize the crosslinking and curing of the photosensitive material and then play the anti-corrosion effect.
- the irradiation time of ultraviolet light in the step S2 is t1 to 1-200s.
- the length of the ultraviolet light irradiation time is closely related to the exposure degree of the base photoresist. If the ultraviolet light irradiation time is too short or too long, the base photoresist will be under-exposed or over-exposed, which will eventually lead to incomplete patterns. accurate. In the range of 1-200s, the substrate photoresist can form the required microchannel network structure on the microfluidic chip after exposure, and beyond this range, the microchannel network structure will be damaged to varying degrees.
- the content of sodium carbonate in the developer is 0.5-3%.
- the sodium carbonate content in the developing solution is 0.5-3%, that is, the developing solution is weakly alkaline, and the unexposed base photoresist (polyvinyl alcohol laurate) is hydrolyzed in a weakly alkaline environment to form water-soluble Polyvinyl alcohol and lauric acid, and the exposed area of the base photoresist after cross-linking and curing is basically not affected by weak alkali, thereby generating a patterned photoresist with clear and complete pattern information.
- the drying temperature T1 is 40-150°C
- the drying time t2 is 0.5-4h.
- the drying temperature is 40-150°C, which can maintain a good drying effect, and can avoid the change of the physical and chemical properties of the polymer due to the high drying temperature, and stabilize the quality of the patterned polymer.
- the temperature T2 of the heating and baking polymer layer is 50-200° C.
- the heating and baking time t3 is 1-4 h.
- the polymer layer is heated within the range of 50-200°C for 1-4h, and the polymer layer is completely crosslinked and cured to form a solid coating with a fixed shape, so that the pattern on the patterned photoresist can be transferred
- the polymer layer on the top surface of the patterned photoresist is dissolved by organic solvents, strong acids or strong alkalis, the polymer layer that is completely crosslinked and cured on the base material will be less affected by the dissolution, thereby ensuring the patterned lithography
- the thinner polymer layer on the top surface of the glue is first dissolved, so that the subsequent release solution can dissolve the patterned photoresist to obtain a patterned polymer.
- step S5 the organic solvent, strong alkali, or strong acid is used to treat the polymer layer by immersion.
- step S5 the organic solvent, strong alkali or strong acid is immersed in the polymer layer, so that the thinner polymer layer on the top surface of the patterned photoresist can be completely immersed and slowly and completely dissolved.
- the dissolution dead angle of the thinner polymer layer on the top surface of the patterned photoresist facilitates the subsequent release liquid to dissolve the patterned photoresist from the polymer layer.
- the release liquid is heated to a temperature T3 of 50-100° C. and then the patterned photoresist and polymer layer are immersed, and the immersion time t4 is 0.5-3h.
- the photoresist (photosensitive material) made of polyvinyl alcohol laurate and other materials is opened by the double bond in the molecule under the action of light, and the chain Cross-link with the chain and solidify to form an insoluble network structure.
- the strong alkaline release solution immersed the crosslinked and cured polyvinyl alcohol laurate to hydrolyze the ester bond in the polyvinyl alcohol lauric acid chain and then break the chain, and finally decompose the insoluble network structure into soluble polyvinyl alcohol Lauric acid.
- the release liquid phase at 50-100°C has better hydrolysis ability for patterned photoresist than cold release liquid, while overheated release liquid is likely to corrode the polymer. Therefore, the temperature of the release liquid is 50- 100°C is most suitable.
- step S5 First coat a polymer layer on the surface of the base material and make the thickness of the polymer layer smaller than the thickness of the patterned photoresist, and then in step S5, after the polymer is leveled and cured, it is treated with an organic solvent, a strong acid or a strong base to make the pattern
- the thinner polymer layer on the top surface of the photoresist slowly dissolves; finally, in step S6, the patterned photoresist is gradually cracked and dispersed by the release liquid, and finally peeled off from the base material to obtain a patterned polymer.
- the separation between polymer and patterned photoresist is converted from traditional stripping to dissolution separation.
- the separation process between polymer and patterned photoresist is more gentle, the patterned polymer structure is not easily damaged, the production quality is higher, and the operation Difficulty, lower requirements for equipment accuracy, operating environment, more stable production quality and more efficient production.
- FIG. 1 is a schematic diagram of the structure of the base photoresist in the S1 step of Embodiment 1-5;
- FIG. 2 is a schematic diagram of the structure of the patterned photoresist in the S3 step of Embodiment 1-5;
- FIG. 3 is a schematic diagram of the structure of the polymer layer in the S4 step of Examples 1-5;
- FIG. 5 is a schematic diagram of the structure of the polymer layer in the S6 step of Examples 1-5;
- Example 6 is a schematic diagram of the structure of the polymer bottom layer in the S0 step of Example 6;
- FIG. 7 is a schematic diagram of the structure of the base photoresist in step S1 of Embodiment 6;
- FIG. 8 is a schematic diagram of the structure of the patterned photoresist in step S3 of Embodiment 6;
- FIG. 10 is a schematic diagram of the structure of the polymer layer in step S5 of Example 6;
- FIG. 11 is a schematic diagram of the structure of the polymer layer in step S6 of Example 6.
- FIG. 11 is a schematic diagram of the structure of the polymer layer in step S6 of Example 6.
- a method for preparing a patterned polymer includes the following steps:
- Spraying photoresist referring to Figure 1, apply a layer of controllable thickness on the flat surface of the base material 1 (such as silicon wafers, glass sheets, plastic sheets, paper sheets, resin sheets, etc.) by spin coating, spraying, etc.
- Base photoresist 2 referring to Figure 1, apply a layer of controllable thickness on the flat surface of the base material 1 (such as silicon wafers, glass sheets, plastic sheets, paper sheets, resin sheets, etc.) by spin coating, spraying, etc.
- Base photoresist 2 referring to Figure 1, apply a layer of controllable thickness on the flat surface of the base material 1 (such as silicon wafers, glass sheets, plastic sheets, paper sheets, resin sheets, etc.) by spin coating, spraying, etc.
- Base photoresist 2 referring to Figure 1, apply a layer of controllable thickness on the flat surface of the base material 1 (such as silicon wafers, glass sheets, plastic sheets, paper sheets, resin sheets, etc.) by spin coating, spraying, etc.
- Pattern transfer referring to Figure 2, make a patterned optical reticle, place the optical reticle on the base photoresist 2 and irradiate the pattern transfer on the optical reticle with ultraviolet light with a wavelength of ⁇ and an illumination intensity of i To the base photoresist 2, the irradiation time is t1;
- Coating polymer Referring to Figure 4, the base material 1 and the patterned photoresist 3 are dried at a temperature of T1, and the drying time is t2. The surface of the base material 1 is coated by spin coating or spraying. Cover a polymer layer 4 with a thickness smaller than that of the patterned photoresist 3, and let it stand until the polymer layer 4 is fully leveled;
- the polymer layer 4 is heated and baked at a temperature of T2 to fully crosslink and solidify, and the heating and baking time is t3, and then pass through organic solvents (acetone, isopropanol, toluene, One of xylene, etc.), strong acid (sulfuric acid, hydrochloric acid, etc.) or strong alkali (sodium hydroxide, potassium hydroxide, etc.) immerses the polymer layer 4 to slowly dissolve the polymer on the top surface of the patterned photoresist 3;
- organic solvents acetone, isopropanol, toluene, One of xylene, etc.
- strong acid sulfuric acid, hydrochloric acid, etc.
- strong alkali sodium hydroxide, potassium hydroxide, etc.
- Photoresist release referring to Figure 6, heat the release solution whose main component is strong alkali (sodium hydroxide, potassium hydroxide, etc.) to a temperature of T3 and then immerse the patterned photoresist 3 and the polymer layer 4 , The immersion time is t4; and then under the action of external force, such as washing, ultrasound, etc., the patterned photoresist 3 is gradually cracked and dispersed into small particles until they fall off to obtain a patterned polymer.
- strong alkali sodium hydroxide, potassium hydroxide, etc.
- Embodiment 1 A method for preparing a patterned polymer.
- the specific operation steps of this embodiment are as described in the above steps S1, S2, S3, S4, S5, and S6, wherein the process parameters in each step are shown in Table 1. Shown.
- Embodiment 2 A method for preparing a patterned polymer.
- the difference between this embodiment and Embodiment 1 is that the process parameters in each step are different, and the specific parameters are shown in Table 1.
- Embodiment 3 A method for preparing a patterned polymer.
- the difference between this embodiment and Embodiment 1 is that the process parameters in each step are different, and the specific parameters are shown in Table 1.
- Embodiment 4 A method for preparing a patterned polymer.
- the difference between this embodiment and Embodiment 1 is that the process parameters in each step are different, and the specific parameters are shown in Table 1.
- Embodiment 5 A method for preparing a patterned polymer.
- the difference between this embodiment and Embodiment 1 is that the process parameters in each step are different, and the specific parameters are shown in Table 1.
- Embodiment 6 A method for preparing a patterned polymer.
- the difference between this embodiment and Embodiment 1 is that before step S1, there is also step S0: first coat a layer of polymer bottom layer 5 on the surface of the base material 1.
- the coating method is the same as in step S4, and the base photoresist 2 is coated on the polymer bottom layer 5.
- the method of separating the polymer from the patterned photoresist 3 is to use a release solution to dissolve the patterned photoresist 3, so that the patterned photoresist 3 is gradually decomposed and dispersed into small particles.
- a release solution to dissolve the patterned photoresist 3, so that the patterned photoresist 3 is gradually decomposed and dispersed into small particles.
- the separation between the polymer and the patterned photoresist 3 is converted from traditional peeling to dissolution separation.
- the separation process between the polymer and the patterned photoresist 3 is smoother, the patterned polymer structure is not easily damaged, and the production quality is better. High, and the operation difficulty, equipment accuracy, operating environment requirements are lower, the production quality is more stable, and the production is more efficient.
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Abstract
一种制备图案化聚合物的方法,为微流控芯片的技术领域,包括以下步骤:S1:喷涂光刻胶;S2:图案转移;S3:显影液显影;S4:涂覆聚合物;S5:溶解聚合物;S6:光刻胶脱模。
Description
本申请要求于2019年7月3日申请的、申请号为201910598079.5、名称为“一种制备图案化聚合物的方法”的中国专利申请的优先权,其全部内容通过引用结合在本申请中。
本申请涉及微流控芯片的技术领域,尤其是涉及一种制备图案化聚合物的方法。
微流控芯片技术是把生物、化学、医学分析过程的样品制备、反应、分离、检测等基本操作单元集成到一块微米尺度的芯片上,自动完成分析全过程。由于它在生物、化学、医学等领域的巨大潜力,已经发展成为一个生物、化学、医学、流体、电子、材料、机械等学科交叉的崭新研究领域。目前,微流控芯片可使用玻璃、聚合物、水凝胶、纸等材料进行加工,但最常见的材料是聚合物。其中,聚合物中广泛使用的是有机硅胶类如聚二甲基硅氧烷(PDMS),其他类型的聚合物如聚甲基丙烯酸甲酯、聚碳酸酯等也有一定的应用。
聚合物性质稳定尤其是有机硅胶类表面能低,因此难以实现高质量的直接光刻图案化加工,而且其工艺中使用大量如甲苯等有机溶剂对环境危害极大。目前的工艺多是采用倒模的间接图案加工方法,该方法首先采用标准的光刻法将图案通过掩板转移至光刻胶如SU-8上,制备出具有厚度和图案的模具。然后,将聚合物浇注在光刻胶制备的模具表面,烘干后从模具上剥离下来,便得到了图案化的聚合物。然而倒模法最后阶段需要将图案化聚合物从光刻胶模具上小心剥离下来,图案化聚合物上微结构众多,在剥离过程中容易受到损坏,对设备、环境要求很高,质量难以把控。
本申请的主要目的是提供一种工艺流程简单、生产质量稳定的制备图案化聚合物的方法。
本申请是通过以下技术方案得以实现的:
一种制备图案化聚合物的方法,其特征在于,包括以下步骤:
S1.喷涂光刻胶:在基底材料表面涂覆一层基底光刻胶;
S2.图案转移:制作有图案的光学掩模版,将光学掩模版放置在基底光刻胶上方并用紫外光照射至光学掩模版上的图案转移至基底光刻胶上;
S3.显影液显影:利用主要成分为碳酸钠的显影液对基底光刻胶进行显影处理,在基底材料上得到图案化光刻胶;
S4.涂覆聚合物:烘干基底材料和图案化光刻胶,在基底材料表面涂覆一层厚度小于图案化光刻胶厚度的聚合物层,静置至聚合物层充分流平;
S5.溶解聚合物:加热烘烤聚合物层至充分交联固化,再通过有机溶剂、强酸或强碱处理聚合物层使图案化光刻胶顶面上的聚合物缓慢溶解;
S6.光刻胶脱模:采用主要成分为强碱的脱膜液处理图案化光刻胶和聚合物层,再冲洗、超声处理得到图案化的聚合物。
通过采用上述技术方案,步骤S2中,紫外光照射放置在基底光刻胶上的光学掩模版时,基底光刻胶的曝光区域交联固化,变成非水溶性的图案化光刻胶并在步骤S3中显影时留下,其余部分被则被冲洗掉,完成第一次图案转印。
然后步骤S4中在基底材料表面涂覆一层聚合物层并使聚合物层厚度小于图案化光刻胶的厚度,再在步骤S5中待聚合物流平固化后通过有机溶剂、强酸或强碱处理,使图案化光刻胶顶面上的较薄聚合物层缓慢溶解;最后在步骤S6中通过脱膜液使图案化光刻胶逐渐裂解分散,最后从基底材料上脱落,实现第二次图案转印,同时得到图案化的聚合物。
最后阶段的聚合物脱模过程中,聚合物与图案化光刻胶的分离方式为通过脱膜液溶解图案化光刻胶,使图案化光刻胶逐渐裂解分散成小颗粒并与聚合物分离,从而得到图案化聚合物。此过程聚合物与图案化光刻胶之间的分离由传统的剥离转换成溶解分离,聚合物与图案化光刻胶的分离过程更加平缓,图案化聚合物结构不易损坏,生产质量更高,且操作难度、对设备精度、操作环境要求更低,生产质量更加稳定、生产更加高效。
进一步设置为:所述S2步骤中,紫外光波长λ范围为315-400nm,光照强度i为0.1-100mW/cm
2。
通过采用上述技术方案,根据光刻胶的化学反应机理和显影原理,基底光刻胶在受到紫外光照射后发生交联固化形成不溶性网状结构的作用机理为:聚乙烯醇月桂酸酯等材料制作的光刻胶(光敏材料)在光的作用下分子中的双键被打开,并使链与链之间发生交联进而固化形成不溶性网状结构。而双键打开需要吸收能量即键能,而光能与光线波长及光照强度有关,因此只有在此波长范围及光照强度范围内的紫外光,其能量才能被双键吸收,进而打开双键,实现光敏材料的交联固化进而起到抗蚀效果。
进一步设置为:所述S2步骤中紫外光的照射时间为t1为1-200s。
通过采用上述技术方案,紫外光的照射时间长短与基底光刻胶的曝光程度密切相关,紫外光照射时间过短或过长,都会使基底光刻胶曝光不充分或过度曝光,最终导致图案不精确。在1-200s范围内,基底光刻胶曝光后可以形成微流控芯片上所需要的微管道网络结构,超出此范围之外,微管道网络结构将受到不同程度破坏。
进一步设置为:所述S3步骤中,显影液中碳酸钠含量为0.5-3%。
通过采用上述技术方案,显影液中碳酸钠含量为0.5-3%,即显影液呈弱碱性,未曝光的基底光刻胶(聚乙烯醇月桂酸酯)在弱碱环境中水解,生成水溶性的聚乙烯醇和月桂酸,而交联固化后的基底光刻胶曝光区域则基本不受弱碱影响,从而生成图案信息清楚完整的图案化光刻胶。
进一步设置为:所述S4步骤中,烘干温度T1为40-150℃,烘干时长t2为0.5-4h。
通过采用上述技术方案,经过显影液处理之后的基底材料上会附着残余的水分,如果不将基底材料和图案化光刻胶烘干,后续涂覆聚合物层时容易导致聚合物层与基底材料之间的附着性和聚合物与图案化光刻胶之间的衔接性不佳,影响图案化聚合物的图案转印质量。烘干温度在40-150℃,可以使保持较好的烘干效果,且可避免由于烘干温度过高引起聚合物物化性质发生转变,稳定图案化聚合物的质量。
进一步设置为:所述S5步骤中,加热烘烤聚合物层的温度T2为50-200℃,加热烘烤时间t3为1-4h。
通过采用上述技术方案,聚合物层在50-200℃范围内受热1-4h,聚合物层完全发生交联固化,形成形状固定的固体涂层,从而可以将图案化光刻胶上的图案转印下来,后期利用有机溶剂、强酸或者强碱溶解图案化光刻胶顶面上的聚合物层时,基底材料上交联固化完全的聚合物层受到溶解影响较小,从而保证图案化光刻胶顶面上的较薄聚合物层首先溶解,便于后续脱膜液溶解图案化光刻胶,得到图案化聚合物。
进一步设置为:所述S5步骤中,有机溶剂或强碱、强酸采用浸没方式处理聚合物层。
通过采用上述技术方案,步骤S5中,有机溶剂、强碱或强酸采用浸没方式处理聚合物层,可以使图案化光刻胶顶面上的较薄聚合物层被完全浸没并缓慢彻底溶解,消除图案化光刻胶顶面上的较薄聚合物层的溶解死角,进而方便后续脱膜液将图案化光刻胶从聚合物层中溶解出来。
进一步设置为:所述S6步骤中,将脱膜液加热至温度T3为50-100℃后再浸没处理图案化光刻胶和聚合物层,浸没时间t4为0.5-3h。
通过采用上述技术方案,根据基底光刻胶的交联固化原理:聚乙烯醇月桂酸酯等材料制作的光刻胶(光敏材料)在光的作用下分子中的双键被打开,并使链与链之间发生交联进而固化形成不溶性网状结构。强碱性脱膜液浸没交联固化后的聚乙烯醇月桂酸酯,使聚乙烯醇月桂酸链中的酯键水解进而发生链中断裂,最终使不溶性网状结构分解成可溶性的聚乙烯醇和月桂酸。50-100℃下的脱膜液相较于冷脱膜液对图案化光刻胶具有更好的水解能力,而过热的脱膜液则容易腐蚀聚合物,因此,脱膜液温度在50-100℃最为适宜。
综上所述,本申请的有益技术效果为:
先在基底材料表面涂覆一层聚合物层并使聚合物层厚度小于图案化光刻胶的厚度,再在步骤S5中待聚合物流平固化后通过有机溶剂、强酸或强碱处理,使图案化光刻胶顶面上的较薄聚合物层缓慢溶解;最后在步骤S6中通过脱膜液使图案化光刻胶逐渐裂解分散,最后从基底材料上脱落,得到图案化的聚合物。聚合物与图案化光刻胶之间的分离由传统的剥离转换成溶解分离,聚合物与图案化光刻胶的分离过程更加平缓,图案化聚合物结构不易损坏,生产质量更高,且操作难度、对设备精度、操作环境要求更低,生产质量更加稳定、生产更加高效。
图1是实施例1-5的S1步骤中的基底光刻胶的结构示意图;
图2是实施例1-5的S3步骤中的图案光刻胶的结构示意图;
图3是实施例1-5的S4步骤中的聚合物层的结构示意图;
图4是实施例1-5的S5步骤中的聚合物层的结构示意图;
图5是实施例1-5的S6步骤中的聚合物层的结构示意图;
图6是实施例6的S0步骤中的聚合物底层的结构示意图;
图7是实施例6的S1步骤中的基底光刻胶的结构示意图;
图8是实施例6的S3步骤中的图案光刻胶的结构示意图;
图9是实施例6的S4步骤中的聚合物层的结构示意图;
图10是实施例6的S5步骤中的聚合物层的结构示意图;
图11是实施例6的S6步骤中的聚合物层的结构示意图。
附图标记:1、基底材料;2、基底光刻胶;3、图案化光刻胶;4、聚合物层;5、聚合物底层。
以下结合附图对本申请作进一步详细说明。
一种制备图案化聚合物的方法,包括以下步骤:
S1.喷涂光刻胶:参照图1,在基底材料1(如硅片、玻璃片、塑料片、纸片、树脂片等)平整表面通过旋涂、喷涂等方式涂覆一层厚度可控的基底光刻胶2;
S2.图案转移:参照图2,制作有图案的光学掩模版,将光学掩模版放置在基底光刻胶2上方并用波长为λ,光照强度为i的紫外光照射至光学掩模版上的图案转移至基底光刻胶2上,照射时间为t1;
S3.显影液显影:参照图3,使用碳酸钠含量为w的D-7显影液浸没或喷涂基底光刻胶2进行显影处理,在基底材料1上得到图案化光刻胶3;
S4.涂覆聚合物:参照图4,在温度为T1的条件下烘干基底材料1和图案化光刻胶3,烘干时长为t2,在基底材料1表面采用旋涂或喷涂等方式涂覆一层厚度小于图案化光刻胶3厚度的聚合物层4,静置至聚合物层4充分流平;
S5.溶解聚合物:参照图5,在温度为T2的条件下加热烘烤聚合物层4至充分交联固化,加热烘烤时长为t3,再通过有机溶剂(丙酮、异丙醇、甲苯、二甲苯等)、强酸(硫酸、盐酸等)或强碱(氢氧化钠、氢氧化钾等)中的一种浸没聚合物层4使图案化光刻胶3顶面上的聚合物缓慢溶解;
S6.光刻胶脱模:参照图6,将主要成分为强碱(氢氧化钠、氢氧化钾等)的脱膜液加热至温度为T3后浸没图案化光刻胶3和聚合物层4,浸没时间为t4;再在外力作用下如冲洗、超声等得到将图案化光刻胶3逐渐裂解分散成小颗粒直至脱落,得到图案化的聚合物。
下面结合具体实施例对本申请作进一步详细说明。
实施例1:一种制备图案化聚合物的方法,本实施例的具体操作步骤如上述步骤S1、S2、S3、S4、S5、S6所述,其中,各个步骤中的各工艺参数如表1所示。
表1实施例1-5各工艺参数数据表
实施例2:一种制备图案化聚合物的方法,本实施例与实施例1的区别在于,各个步骤中的工艺参数不同,具体参数如表1所示。
实施例3:一种制备图案化聚合物的方法,本实施例与实施例1的区别在于,各个步骤中的工艺参数不同,具体参数如表1所示。
实施例4:一种制备图案化聚合物的方法,本实施例与实施例1的区别在于,各个步骤中的工艺参数不同,具体参数如表1所示。
实施例5:一种制备图案化聚合物的方法,本实施例与实施例1的区别在于,各个步骤中的工艺参数不同,具体参数如表1所示。
实施例6:一种制备图案化聚合物的方法,本实施例与实施例1的区别在于,在步骤S1之前,还有步骤S0:先在基底材料1表面涂覆一层聚合物底层5,涂覆方式与步骤S4相同,基底光刻胶2涂覆在聚合物底层5上。
本实施例的实施原理及有益效果为:聚合物与图案化光刻胶3的分离方式为采用脱膜液溶解图案化光刻胶3,使图案化光刻胶3逐渐裂解分散成小颗粒并与聚合物分离,从而得到图案化聚合物。此过程聚合物与图案化光刻胶3之间的分离由传统的剥离转换成溶解分离,聚合物与图案化光刻胶3的分离过程更加平缓,图案化聚合物结构不易损坏,生产质量更高,且操作难度、对设备精度、操作环境要求更低,生产质量更加稳定、生产更加高效。
本具体实施方式的实施例均为本申请的较佳实施例,并非依此限制本申请的保护范围,故:凡依本申请的结构、形状、原理所做的等效变化,均应涵盖于本申请的保护范围之内。
Claims (8)
- 一种制备图案化聚合物的方法,包括以下步骤:S1.喷涂光刻胶:在基底材料表面涂覆一层基底光刻胶;S2.图案转移:制作有图案的光学掩模版,将光学掩模版放置在基底光刻胶上方并用紫外光照射至光学掩模版上的图案转移至基底光刻胶上;S3.显影液显影:利用主要成分为碳酸钠的显影液对基底光刻胶进行显影处理,在基底材料上得到图案化光刻胶;S4.涂覆聚合物:烘干基底材料和图案化光刻胶,在基底材料表面涂覆一层厚度小于图案化光刻胶厚度的聚合物层,静置至聚合物层充分流平;S5.溶解聚合物:加热烘烤聚合物层至充分交联固化,再通过有机溶剂、强酸或强碱处理聚合物层使图案化光刻胶顶面上的聚合物缓慢溶解;S6.光刻胶脱模:采用主要成分为强碱的脱膜液处理图案化光刻胶和聚合物层,再冲洗、超声处理得到图案化的聚合物。
- 根据权利要求1所述的制备图案化聚合物的方法,其中,所述S2步骤中,紫外光波长λ范围为315-400nm,光照强度i为0.1-100mW/cm 2。
- 根据权利要求1或2所述的制备图案化聚合物的方法,其中,所述S2步骤中紫外光的照射时间为t1为1-200s。
- 根据权利要求1所述的制备图案化聚合物的方法,其中,所述S3步骤中,显影液中碳酸钠含量为0.5-3%。
- 根据权利要求1所述的制备图案化聚合物的方法,其中,所述S4步骤中,烘干温度T1为40-150℃,烘干时长t2为0.5-4h。
- 根据权利要求1所述的制备图案化聚合物的方法,其中,所述S5步骤中,加热烘烤聚合物层的温度T2为50-200℃,加热烘烤时间t3为1-4h。
- 根据权利要求1或6所述的制备图案化聚合物的方法,其中,所述S5步骤中,有机溶剂或强碱、强酸采用浸没方式处理聚合物层。
- 根据权利要求1所述的制备图案化聚合物的方法,其中,所述S6步骤中,将脱膜液加热至温度T3为50-100℃后再浸没处理图案化光刻胶和聚合物层,浸没时间t4为0.5-3h。
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