本文關(guān)鍵詞： 微全分析系統(tǒng)芯片 混沌微混合器 多層芯片鍵合 重金屬檢測(cè)　出處：《哈爾濱工業(yè)大學(xué)》2015年博士論文　論文類型：學(xué)位論文

【摘要】：基于微電子機(jī)械系統(tǒng)(Micro Electro Mechanical System,MEMS)技術(shù)的微全分析系統(tǒng)(Micro total analysis systems,μTAS)是微電子、電化學(xué)、及分析化學(xué)等多學(xué)科交叉結(jié)合的產(chǎn)物,由于具有廣闊的應(yīng)用前景而成為研究的熱點(diǎn)。然而目前用于水質(zhì)重金屬污染檢測(cè)的μTAS芯片還存在預(yù)處理效率低、多層芯片鍵合難等問(wèn)題,導(dǎo)致其集成程度并不高,無(wú)法滿足便攜化和實(shí)時(shí)化檢測(cè)需求。本文提出了三維馬蹄混沌混合器結(jié)構(gòu),以改善預(yù)處理效率;以微混合器為核心,結(jié)合固相萃取及安培檢測(cè)技術(shù),設(shè)計(jì)了集成化的重金屬μTAS芯片;提出了基于聚甲基丙烯酸甲酯(PolymethylMethacrylate,PMMA)材料的新穎鍵合方法,以實(shí)現(xiàn)帶有功能模塊的多層復(fù)雜μTAS芯片的組裝;基于以上設(shè)計(jì)和裝配工藝,制備了重金屬μTAS芯片,并采用多種檢測(cè)方法對(duì)芯片的性能進(jìn)行了驗(yàn)證。提出了三維馬蹄變換模型,通過(guò)“垂直折疊”使二維馬蹄變換后“溢出”的流體再次回到系統(tǒng)內(nèi)部,不僅減少了變換過(guò)程中的流體損失,而且流動(dòng)方向的多次改變使得混合器內(nèi)的流動(dòng)情況更加復(fù)雜。以流體動(dòng)力學(xué)方程和多組分物質(zhì)擴(kuò)散方程為基礎(chǔ),建立了微尺度下的流體混合模型,研究了混沌混合器的性能,結(jié)果表明變換后混沌流對(duì)混合的促進(jìn)作用更為顯著。當(dāng)Re=10時(shí)經(jīng)優(yōu)化設(shè)計(jì)后的三維馬蹄微混合器在12mm的混合距離內(nèi)即可接近均勻混合(σ0.05),與“擠回式”馬蹄混合器(Re=10,σ0.2)相比混合效果得到了明顯改善。以微混合器為核心,設(shè)計(jì)了新穎的重金屬μTAS芯片集成結(jié)構(gòu)。利用三維馬蹄混合器對(duì)試樣進(jìn)行預(yù)處理,以滿足固相萃取柱的選擇性吸附條件;設(shè)計(jì)一體化的填充式柱床結(jié)構(gòu),結(jié)合改性吸附劑實(shí)現(xiàn)對(duì)重金屬離子的分離富集;在流經(jīng)式檢測(cè)池結(jié)構(gòu)的基礎(chǔ)上設(shè)計(jì)了帶有內(nèi)充液池的Ag/Ag Cl參比電極,保證重金屬安培檢測(cè)的穩(wěn)定性。芯片由4層基片組成,整體尺寸為70mm×40mm×14mm,除壓力進(jìn)樣裝置和電化學(xué)工作站外,整個(gè)檢測(cè)過(guò)程無(wú)需借助其他外部設(shè)備,使μTAS芯片的集成化程度得到了顯著提高。為實(shí)現(xiàn)基于PMMA材料的多層復(fù)雜結(jié)構(gòu)μTAS芯片的裝配,提出了有機(jī)溶劑混溶浸泡鍵合法。把三氯甲烷與無(wú)水乙醇按照一定比例混合,通過(guò)調(diào)節(jié)溶液組成和浸泡時(shí)間等參數(shù)控制材料形變量,在保證微結(jié)構(gòu)形貌的前提下實(shí)現(xiàn)了芯片的封合。當(dāng)浸泡鍵合條件為:V三氯甲烷:V乙醇=1:10、t=10 min、T=40°C時(shí),鍵合強(qiáng)度達(dá)到了267.5N/cm~2而形變量只有7.26%。為解決帶有功能模塊的μTAS芯片的裝配,提出了有機(jī)溶劑熏蒸鍵合法。利用聚酰亞胺和硅膠作為掩膜,保護(hù)功能模塊中易受有機(jī)蒸汽破壞的部分,當(dāng)使用三氯甲烷作為熏蒸溶劑、熏蒸溫度為65°C、熏蒸時(shí)間為40s時(shí),鍵合強(qiáng)度為61N/cm~2,形變量為9.5%。使用以上裝配方法,分別制作了用于試樣預(yù)處理的微混合器芯片、用于重金屬離子分離的固相萃取芯片和用于重金屬離子檢測(cè)的安培傳感器芯片,并采用多種測(cè)試方法對(duì)上述芯片的性能進(jìn)行了評(píng)價(jià)。以此為依據(jù)確定了μTAS芯片的工作條件。最后以Hg~（2+）溶液和Pb~（2+）、Cr~（3+）混合溶液作為模擬試樣,對(duì)μTAS芯片進(jìn)行了整體性能測(cè)試。芯片對(duì)Hg~（2+）離子的檢出限為20μg/L,(n=5,標(biāo)準(zhǔn)差3%);當(dāng)有高濃度干擾離子時(shí)(Cr~（3+）=1.0×10-6 mol/L),芯片仍可實(shí)現(xiàn)對(duì)濃度為1mg/L的Pb~（2+）離子準(zhǔn)確檢出,兩項(xiàng)指標(biāo)均滿足我國(guó)現(xiàn)行污水綜合排放標(biāo)準(zhǔn)(GB8978-1996)中對(duì)金屬汞(50μg/L)和金屬鉛(1mg/L)的檢測(cè)要求。
[Abstract]:Based on micro electro mechanical system (Micro Electro Mechanical System, MEMS) micro total analysis system technology (Micro total analysis systems, TAS) is the product of microelectronics, electrochemistry, chemical analysis and interdisciplinary combination, because of its wide application and become a research hotspot. However, for TAS chip detection of heavy metal pollution there are water pretreatment efficiency is low, multilayer chip bonding and other difficult issues, the integration degree is not high, can not meet the demand of portable and real-time detection. This paper proposes a three-dimensional horseshoe mixed structure chaotic mixer, in order to improve the efficiency of pretreatment; micro mixer as the core, combined with solid phase extraction and amperometric detection technology. The design of the heavy metal TAS chip integrated; based on poly (PolymethylMethacrylate, PMMA) for new key materials, in order to achieve a power Multi module complex assembly TAS chip; the design and assembly process based on TAS chip, heavy metals were prepared, and using a variety of detection methods on the performance of the chip is verified. The 3D horseshoe model, through the "vertical folding" to transform two-dimensional horseshoe fluid "overflow" again within the system, not only reduces the loss of fluid in the process of transformation, and the flow direction of the flow in the mixer makes many changes more complex. As the fluid dynamics equations and multicomponent diffusion equation as the foundation, established a mixed fluid model in micro scale, the research results show that the performance of chaotic mixer, chaos transform the flow of mixed effect is more significant. When Re=10 by 3D horseshoe optimization design of the micro mixer can be mixed in the distance 12mm near uniform mixture (sigma 0.05), and "Push back" horseshoe mixer (Re=10, sigma 0.2) compared to the mixing effect has been improved. The micro mixer design as the core, the heavy metal TAS chip integrated with new structure. The samples were pretreated by using three-dimensional horseshoe mixer, to meet the selection of adsorption conditions of solid phase extraction column; column type filling structure the integrated design, combined with the modified adsorbent to achieve the separation of the enrichment of heavy metal ions; based on flow-through detection pool structure on the design of the pool with liquid filling within the Ag/Ag Cl reference electrode, ensure the stability of heavy metal. The chip amperometric detection consists of 4 layers of substrate, the overall size is 70mm * 40MM * 14mm. In addition to the pressure sampling device and electrochemical workstation, the whole testing process without the help of other external devices, the integration degree of TAS chip has been greatly improved. In order to realize the complex structure of multilayer PMMA material based on TAS Chip assembly, proposed miscible organic solvent immersion bonding. The chloroform and ethanol are mixed according to a certain proportion, by adjusting the composition of solution and soaking time parameters of material deformation control, in the premise of the micro structure and morphology of the chip to achieve sealing. When immersion bonding conditions are as follows: V chloroform: V =1:10 t=10 min, T=40 ethanol, C, the bonding strength reached 267.5N/cm~2 and 7.26%. as the only variable assembly to solve TAS chip with the function module, the organic solvent bonding method. Using the fumigation of polyimide and silica gel as a mask, vulnerable to destruction of organic vapor partial protection module, when using chloroform as solvent fumigation, fumigation temperature is 65 ~ C, fumigation time is 40s, the bonding strength is 61N/cm~2, the shape variables for 9.5%. using the above method of assembly, we fabricated the sample pretreatment for the micro Mixer chip, chip used for solid phase extraction and separation of heavy metal ions for amperometric detection of heavy metal ion sensor chip, and uses a variety of testing methods on the performance of the chip was evaluated. In order to determine the TAS chip working conditions as the basis. Finally, using Hg~ (2+) solution and Pb~ (2+), Cr~ (3+) mixed solution as simulated specimens of TAS chip for the overall performance test. The chip of Hg~ (2+) ion detection limit was 20 (g/L, n=5, standard deviation 3%); when there is a high concentration of interference ions (Cr~ (3+) =1.0 * 10-6 mol/L), the concentration of 1mg/L can be realized on chip Pb~ (2+) ion detection, two indicators are meet the integrated wastewater discharge standard of China (GB8978-1996) of mercury (50 g/L) and lead (1mg/L) detection requirements.

【學(xué)位授予單位】：哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2015
【分類號(hào)】：TN40;TH-39

【相似文獻(xiàn)】

相關(guān)期刊論文 前10條

1 王偉;范大和;;分析化學(xué)領(lǐng)域的新興學(xué)科-微全分析系統(tǒng)[J];鹽城工學(xué)院學(xué)報(bào)(自然科學(xué)版);2007年02期

2 林炳承;微全分析系統(tǒng)中的微分離學(xué)及其在生命科學(xué)中的應(yīng)用[J];現(xiàn)代科學(xué)儀器;2001年04期

3 劉繼鋒,曹衛(wèi)東,汪爾康;電化學(xué)檢測(cè)微全分析系統(tǒng)[J];現(xiàn)代科學(xué)儀器;2001年02期

4 張效偉;;基于電滲驅(qū)動(dòng)電磁閥切換恒電位檢測(cè)的微全分析系統(tǒng)[J];儀表技術(shù)與傳感器;2013年08期

5 金欽漢;從2001年P(guān)ITTCON看微全分析系統(tǒng)的發(fā)展[J];現(xiàn)代科學(xué)儀器;2001年04期

6 崔大付;微全分析系統(tǒng)中的MEMS技術(shù)[J];現(xiàn)代科學(xué)儀器;2001年04期

7 方肇倫;;微全分析系統(tǒng)——分析儀器的方向與前沿[J];科學(xué)新聞;2001年01期

8 陳超,趙湛,張搏軍;基于線陣電極電泳芯片的微全分析系統(tǒng)[J];微納電子技術(shù);2003年Z1期

9 于建群,王立鼎,劉軍山,郭麗莎;塑料電泳芯片微結(jié)構(gòu)模壓的試驗(yàn)研究[J];機(jī)械工程學(xué)報(bào);2004年11期

10 ;[J];;年期

相關(guān)會(huì)議論文 前1條

1 陳纘光;王立世;莫金垣;;微全分析系統(tǒng)專用微型電源的研制[A];第二屆全國(guó)微全分析系統(tǒng)學(xué)術(shù)會(huì)議論文摘要集[C];2004年

相關(guān)重要報(bào)紙文章 前1條

1 張家駒;應(yīng)大力發(fā)展微全分析系統(tǒng)[N];中國(guó)工業(yè)報(bào);2003年

相關(guān)博士學(xué)位論文 前1條

1 張賀;基于微混合器的重金屬離子微全分析系統(tǒng)芯片研究[D];哈爾濱工業(yè)大學(xué);2015年

相關(guān)碩士學(xué)位論文 前3條

1 任明遠(yuǎn);微全分析系統(tǒng)中的化學(xué)發(fā)光檢測(cè)系統(tǒng)[D];哈爾濱工業(yè)大學(xué);2007年

2 梁寧;微全分析系統(tǒng)中共焦激光誘導(dǎo)熒光檢測(cè)器的研制[D];清華大學(xué);2003年

3 徐明波;SPR技術(shù)在生化分析中的應(yīng)用[D];華中師范大學(xué);2007年

，

本文編號(hào)：1449696