發(fā)布時間：2018-05-18 06:05

  本文選題：無機全固態(tài)電致變色器件 + 反應(yīng)磁控濺射��； 參考：《中國建筑材料科學(xué)研究總院》2017年碩士論文

【摘要】：電致變色材料能夠在外加電壓的條件下通過陽離子和電子的注入與抽出實現(xiàn)自身光學(xué)性能的可逆變化。NiO_x是一種典型的陽極電致變色材料,與其他陽極變色材料相比,NiO_x在循環(huán)壽命和著色效率等方面具有很大的優(yōu)勢,但存在褪色態(tài)透過率低、鋰離子存儲量難與陰極變色層匹配等問題,限制了其在器件中的應(yīng)用。國外的研究已經(jīng)證明,鎢元素摻雜能夠改善NiO_x的性能,但在大多數(shù)關(guān)于W摻雜NiO_x薄膜的研究中,樣品的制備采用共濺射法,在固定Ar/O2比例的條件下進行,缺少關(guān)于氬氧比、工作氣壓等工藝參數(shù)對薄膜影響的研究,并且共濺射不適合大面積規(guī)模化鍍膜生產(chǎn)。本文利用直流反應(yīng)磁控濺射技術(shù),使用摩爾比4:1的鎳鎢合金靶材,在不同的工藝條件下制備NiO_x:W薄膜,研究氬氧比和工作氣壓等反應(yīng)磁控濺射鍍膜工藝對薄膜成分價態(tài)、形貌結(jié)構(gòu)以及性能的影響。此外,Li+是參與電致變色化學(xué)反應(yīng)的必要物質(zhì)之一,鋰化是將Li+引入器件的過程,本課題將尋找合適的鋰化工藝,并以NiO_x:W為陽極層,嘗試制備無機全固態(tài)電致變色器件。反應(yīng)磁控濺射制備獲得的NiO_x:W薄膜由NiO、Ni_2O_3和WO_3的混合物組成。固定工作氣壓不變,增加鍍膜過程中的氧氣流量,薄膜中WO_3含量上升,沉積速率降低,顆粒尺寸減小。薄膜的結(jié)晶程度因面心立方結(jié)構(gòu)的Ni O減少,無定形態(tài)的Ni_2O_3含量上升而降低,NiO的晶格常數(shù)因W6+與Ni2+發(fā)生置換而增大。同時,因Ni2+被氧化形成更多的Ni3+,薄膜的光學(xué)透過率下降,光學(xué)帶隙整體上隨氧分壓上升而減小。由光譜橢偏測試擬合分析獲得NiO_x:W薄膜折射率(λ600 nm)和消光系數(shù)隨氧分壓上升而增大。固定鍍膜過程中的氬氧比不變,工作氣壓上升,樣品中NiO含量上升,但面心立方結(jié)構(gòu)的NiO轉(zhuǎn)變?yōu)榉蔷B(tài),薄膜的結(jié)晶程度降低。隨工作氣壓增大,薄膜表面上的縫隙增多,結(jié)構(gòu)更為疏松。由于Ni2+占鎳元素總量的比例增加及薄膜致密程度的變化,樣品的透射率隨工作氣壓增大而上升。光學(xué)帶隙以及由光譜橢偏法分析得到的折射率和消光系數(shù),總體上都隨工作氣壓增大而提高。鋰化程度對器件的驅(qū)動電壓、著色效率以及光調(diào)制幅度有顯著的影響。制備的器件FTO/LiyWO_3/電解質(zhì)層/NiO_x:W/ITO在波長550nm處著色態(tài)透過率為3.9%,褪色態(tài)透過率為60.2%,光調(diào)制幅度達到56.3%,著色效率為1.54cm2/C。
[Abstract]:Electrochromic materials can realize the reversible change of their optical properties through the implantation and extraction of cations and electrons under the condition of applied voltage. NiOx is a typical anodic electrochromic material. Compared with other anodic discoloration materials, nio _ x has a great advantage in cycle life and coloring efficiency, but it has some problems such as low fading state transmittance and difficult matching of lithium ion storage with cathode chromotropic layer, which limits its application in devices. It has been proved that tungsten doping can improve the properties of NiO_x. However, in most of the studies on W doped NiO_x films, the sample was prepared by co-sputtering under the condition of fixed Ar/O2 ratio, and the ratio of argon to oxygen was missing. The influence of working pressure and other technological parameters on the film is studied, and co-sputtering is not suitable for large-scale coating production. In this paper, NiO_x:W thin films were prepared by DC reactive magnetron sputtering (RMC) with the target material of Nickel-tungsten alloy at 4:1 molar ratio under different technological conditions. The valence states of the films were studied by reactive magnetron sputtering process, such as argon / oxygen ratio and working pressure. The influence of morphology, structure and properties. In addition, Li is one of the necessary substances to participate in electrochromic chemical reaction. Lithium is the process of introducing Li into the device. In this paper, we will find a suitable lithiation process and try to fabricate the inorganic all-solid-state electrochromic device with NiO_x:W as anode layer. The NiO_x:W thin films prepared by reactive magnetron sputtering are composed of NiO _ 2O _ 3 and WO_3. When the working pressure is constant, the oxygen flow rate increases, the WO_3 content in the film increases, the deposition rate decreases and the particle size decreases. The crystalline degree of the thin films decreases due to the decrease of nio in face-centered cubic structure, the increase of amorphous Ni_2O_3 content and the decrease of lattice constant of nio due to the substitution of W _ 6 and Ni2. At the same time, as Ni2 is oxidized to form more Ni3, the optical transmittance decreases, and the optical band gap decreases with the increase of oxygen partial pressure. The refractive index (位 600nm) and extinction coefficient of NiO_x:W thin films are obtained by the fitting analysis of spectroscopic ellipsometry, and the extinction coefficient increases with the increase of oxygen partial pressure. In the fixed coating process, the argon / oxygen ratio is constant, the working pressure increases, the NiO content in the sample increases, but the NiO with face-centered cubic structure changes to amorphous state, and the crystallinity of the film decreases. With the increase of the working pressure, the gap on the surface of the film increases and the structure becomes more loose. Due to the increase of the ratio of Ni2 to the total nickel element and the change of the densification of the film, the transmittance of the sample increases with the increase of the working pressure. The optical band gap and the refractive index and extinction coefficient obtained by spectroscopic ellipsometry increase with the increase of the working pressure. The degree of lithiation has a significant effect on the driving voltage, coloring efficiency and optical modulation amplitude of the device. The FTO/LiyWO_3/ electrolyte layer / NiOx: W / ITO has a coloring state transmittance of 3.9 at wavelength 550nm, a fading state transmittance of 60.2, a light modulation amplitude of 56.3 and a coloring efficiency of 1.54 cm ~ 2 / C.
【學(xué)位授予單位】：中國建筑材料科學(xué)研究總院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TN383.1;TB383.2

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