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面向生物醫學的壓電微機械超聲換能器設計與制備研究

添加時間:2021/11/26 來源:未知 作者:樂楓
擁有良好壓電響應且制備工藝已非常成熟的鋯鈦酸鉛(PZT)薄膜依然是當前十分重要的 PMUT 核心壓電材料,此外,研究人員發現在具有高聲速、溫度穩定性好、寬帶隙等優勢的氮化鋁(AlN)薄膜中摻雜Ⅲ族過渡金屬元素鈧(Sc)能夠明顯改善其自身壓電性能,這對 PMU
以下為本篇論文正文:

摘 要

  隨著超聲波傳感器產業的發展趨勢向微小型化、高集成度、低成本、高性能轉變,基于微機電系統(Microelectromechanical Systems)的超聲換能器應運而生。其中,具有幾何結構簡單、低阻抗、易集成等優勢的壓電式微機械超聲換能器(Piezoelectric Micromachined Ultrasonic Transducer,PMUT)成為近年來研究的熱點,并在生物醫學超聲成像方面有著重大應用價值。隨著超聲成像需求的不斷提高,具有更高分辨率的高頻超聲換能器成為當下和未來的發展方向,這就需要PMUT 單元尺寸在微米尺度,具有良好的幾何結構,并且采用高性能壓電薄膜材料。擁有良好壓電響應且制備工藝已非常成熟的鋯鈦酸鉛(PZT)薄膜依然是當前十分重要的 PMUT 核心壓電材料,此外,研究人員發現在具有高聲速、溫度穩定性好、寬帶隙等優勢的氮化鋁(AlN)薄膜中摻雜Ⅲ族過渡金屬元素鈧(Sc)能夠明顯改善其自身壓電性能,這對 PMUT 產業領域有著巨大吸引力;谏鲜霰尘,本論文主要針對基于 PZT 薄膜和 Sc 摻雜 AlN(ScxAl1-xN)薄膜的 PMUT展開研究,進行了如下四個方面的研究工作:

 。1)研究了 Pt/Ti/SiO2/Si 襯底上 PZT 薄膜的晶體結構及電學性能,結果表明該 PZT 薄膜結構致密,常溫下在 1 kHz 頻率時損耗僅有 0.027,通過壓電力顯微鏡對 PZT 薄膜微區進行表征,薄膜表現出良好的壓電響應。然后,研究了Mo/SiO2/SOI 襯底上 Sc 含量為 29%的 Sc0.29Al0.71N 薄膜的晶體結構及其在高壓的演化,結果表明 Sc0.29Al0.71N 薄膜各層分界清晰,通過電子衍射圖分析得到薄膜表現為六方相多晶薄膜,并計算得到其晶格參數 a 和 c 分別為 3.0997 ? 和 4.9569?.此外,還研究了 Sc 元素在 Sc0.29Al0.71 薄膜中的結合形式以及 Sc0.29Al0.71 薄膜的晶體結構在高壓下的演變行為,Sc0.29Al0.71 薄膜在 20 GPa 的高壓下并沒有產生纖鋅礦到巖鹽礦的相變,這表明該薄膜具有較強的耐高壓特性。

 。2)采用有限元方法(Finite Element Method,FEM)建立了基于 PZT 薄膜的三維 PMUT 仿真模型,在(0,1)模態下,研究 PMUT 壓電薄膜厚度和尺寸、頂部電極直徑和形狀、底部空腔直徑和形狀、襯底頂層硅厚度等一系列幾何參數對PMUT 諧振頻率、靜態靈敏度、有效機電耦合系數(????eff2 )等性能的影響,實現了性能調控,研究發現底部空腔直徑和頂層硅厚度能夠對 PMUT 的諧振頻率和靜態靈敏度產生較為深刻的影響。此外,還對水域下 PMUT 模型的動態傳輸接收特性進行了模擬仿真,經幾何優化后獲得了基于 PZT 薄膜的高頻 PMUT 三維有限元模型,其諧振頻率可達 22.12 MHz,有效機電耦合系數為 5.13%,當反射物距離 PMUT 表面中心 300 μm 處時,相對脈沖回波靈敏度級約為-44.7 dB.

 。3)建立了基于 Sc0.29Al0.71 薄膜的 PMUT 三維有限元模型,經過幾何優化后的 PMUT 模型其諧振頻率可達 23.565 MHz,有效機電耦合系數為 2.5%,當反射物距離 PMUT 表面中心 300 μm 處時,相對脈沖回波靈敏度級約為-50.3 dB.

  此外,還嘗試將沿[011]方向極化的 0.70Pb(Mg1/3Nb2/3)O3-0.30PbTiO3 (PMN-0.30PT)單晶薄膜應用于 PMUT 有限元模型中,探索了在不同頂部電極和底部空腔形狀配置下的 PMUT 模型性能表現。研究發現,這種新型壓電材料以及新型幾何結構為今后實現 PMUT 性能的提升提供了可能。

 。4)根據 PMUT 建模仿真幾何優化后的結構參數制備獲得了基于 PZT 薄膜 PMUT 單元及 50×50 陣列原型器件并進行表征測試。結果顯示 PMUT 單元底部空腔刻蝕情況良好,成功檢測到 PMUT 單元器件(0,1)模態下的諧振頻率為 25.87 MHz,根據脈沖回波測試得到回波信號最大幅值為 4.14 mV.本論文制備出的 PMUT 原型器件有望滿足高分辨率生物醫學超聲成像應用的高頻需求。

  關鍵詞: PMUT;PZT 薄膜;ScxAl1-xN 薄膜;有限元仿真

  Abstract

  As the development trend of the ultrasonic sensor industry shifts to  microminiaturization, high integration, low cost, and high performance, ultrasonic  transducers based on Microelectromechanical Systems (MEMS) have emerged. Among  them, the Piezoelectric Micromachined Ultrasonic Transducer (PMUT), which has the  advantages of simple geometric structure, low impedance, and easy integration, has  become a research hotspot in recent years, and has great application value in biomedical  ultrasound imaging. As the demand for ultrasound imaging continues to increase, high-  frequency ultrasound transducers with higher resolution have become the current and  future development direction. This requires the PMUT unit size to be on the micron  scale, with a good geometric structure, and to use high-performance piezoelectric thin  film. Lead zirconate titanate (PZT) thin film with good piezoelectric response and  mature preparation process is still the current important PMUT core piezoelectric  material. In addition, the researchers found that doping group III transition metal  element scandium (Sc) in aluminum nitride (AlN) film with the advantages of high  sound velocity, good temperature stability, and wide band gap can significantly improve  its own piezoelectric properties, which has great appeal to the PMUT industry. Based  on the above background, this thesis mainly focuses on PMUT based on PZT film and  Sc-doped AlN (ScxAl1-xN) film, and has conducted the following three aspects of  research work:

 。1) The crystal structure and electrical properties of the PZT thin film on  Pt/Ti/SiO2/Si substrate were studied. The results showed that the PZT thin film had a  compact structure, and the loss was only 0.027 at a frequency of 1 kHz at room  temperature. The PZT thin film micro-domains were characterized by a piezoelectric  force microscope, and the thin film showed a good piezoelectric response. Then, the  crystal structure of Sc0.29Al0.71N thin film with a Sc content of 29% on Mo/SiO2/SOI  substrate and its changes under high pressure were studied. The results revealed that  Abstract Shanghai Normal University of Master Philosophy  the boundaries of each layer of the Sc0.29Al0.71N thin film were clear. The electron  diffraction pattern analysis showed that the thin film appeared to be a hexagonal  polycrystalline film. The lattice parameters a and c of Sc0.29Al0.71N thin film were  calculated to be 3.0997 ? and 4.9569 ?, respectively. In addition, the combination of  Sc element in the Sc0.29Al0.71N thin film and the evolution behavior of the crystal  structure of the Sc0.29Al0.71N thin film under high pressure was studied. There was no  wurtzite to rock salt ore phase transition under the high pressure of 20 GPa, indicating  that the film has strong high-pressure resistance.

 。2) The finite element method (Finite Element Method, FEM) was used to  establish three-dimensional PMUT simulation model based on PZT thin film. In the  (0,1) mode, the influence of a series of geometric parameters such as the thickness and  size of the PMUT piezoelectric film, the diameter and shape of the top electrode, the  diameter and shape of the bottom cavity, and the thickness of the silicon on the top of  the substrate, on the resonance frequency, static sensitivity, effective electromechanical  coupling coefficient (eff2 ) and other performance effects of the PMUT were studied.  The performance control was achieved. The study found that the bottom cavity diameter  and the top silicon thickness can have a profound impact on the resonant frequency and  static sensitivity of the PMUT. In addition, the dynamic transmission and reception  characteristics of the PMUT model under water are also simulated. After geometric  optimization, the three-dimensional finite element model of high-frequency PMUT  based on PZT thin film was obtained. Its resonant frequency can reach 22.71 MHz, and  the effective electromechanical coupling coefficient is 5.13%. When the reflector is 300  μm away from the center of the PMUT surface, the relative pulse echo sensitivity levelis about -44.7 dB.

 。3) A three-dimensional finite element model of PMUT was established based on  Sc0.29Al0.71 thin film. The resonant frequency of the PMUT model can reach 23.565  MHz, and the effective electromechanical coupling coefficient is 2.5%, after geometric  optimization. When the reflector is 300 μm away from the center of the PMUT surface,  the relative pulse echo sensitivity level is about -50.3 dB. In addition, an attempt was  made to apply [011] poled 0.70Pb(Mg1/3Nb2/3)O3-0.30PbTiO3 (PMN-0.30PT) thin film  to the PMUT finite element model, the performance of the PMUT model under different  top electrode and bottom cavity shape configurations was explored. The study found  that this new piezoelectric material and new geometric structure provide the possibility  to realize the improvement of PMUT performance in the future.  Shanghai Normal University of Master Philosophy Abstract

 。4) According to the optimized structural parameters of the PMUT modeling and  simulation geometry, the PMUT unit and the 50×50 array prototype devices based on  the PZT thin film were obtained and characterized. The results show that the cavity at  the bottom of the PMUT unit is well etched. It is successfully detected that the  resonance frequency of the PMUT unit device (0,1) mode is 25.87 MHz. The relative  pulse echo sensitivity level is calculated by the pulse echo result to be about -58.5 dB.  The PMUT prototype device prepared in this thesis is expected to meet the high-  frequency requirements of high-resolution biomedical ultrasound imaging applications.

  Keywords: PMUT; PZT thin film; ScxAl1-xN thin film; FEM simulation

  目錄

  第 1 章 緒論

  1.1 引言

  法國科學家 Paul Langevin 在 1917 年第一次使用了石英晶體制作的超聲換能器,同時采用超聲對水下目標進行探測,并將該方法稱為"水下定位法".這時,超聲已作為工程技術出現[1].在過去的幾十年里,超聲波技術已經越來越廣泛地在工業和生物醫學中應用,例如醫學成像,指紋傳感,無損評估,粒子和細胞操縱[2-6].超聲波傳感器利用超聲波換能器來實現聲學和電學信號轉換。隨著對超聲成像領域需求的不斷提高,基于微機電系統(Microelectromechanical Systems,簡 稱 MEMS ) 的 超 聲 換 能 器 應 運 而 生 , 它 被 稱 為 微 機 械 超 聲 換 能 器(Micromachined Ultrasonic Transducer,簡稱 MUT),相比于傳統超聲換能器,MUT 易于陣列化、集成化,具有微小型、更好的聲耦合、更低的功耗等優勢,近年來在醫學超聲成像和指紋傳感領域開始得到了廣泛的應用,MUT 已成為傳統超聲換能器的一種很有前途的替代方案。

  一般來說,根據工作原理的不同,MUT 可分為兩類:電容式微機械超聲換能器(Capacitive Micromachined Ultrasonic Transducer,簡稱 CMUT)和壓電式微機械超聲換能器(Piezoelectric Micromachined Ultrasonic Transducer,簡稱 PMUT)[7].其中,采用壓電材料的正、逆壓電效應工作原理的 PMUT 是近年來研究熱點。

  隨著新型壓電材料的誕生與發展,基于新型幾何結構和壓電材料的 PMUT 為其應用開闊了市場,促使微小型化、高集成度、高性能、低成本成為智能超聲波傳感技術發展的新方向。因此,本論文將圍繞面向生物醫學成像的 PMUT 展開設計與制備方面的研究。

  1.2 微機械超聲換能器的研究概述

  1.2.1 微機電系統簡介

  1.2.2 電容式微機械超聲換能器簡介

  1.2.3 壓電式微機械超聲換能器簡介

  1.3 生物醫學超聲成像概述

  1.3.1 超聲成像原理與技術

  1.3.2 超聲脈沖回波法

  1.4 壓電材料的研究概述

  1.4.1 壓電效應

  1.4.2 壓電方程

  1.4.3 PMUT 壓電材料的選擇

  1.5 問題的提出與研究內容

  1.5.1 問題的提出

  1.5.2 研究內容

  第 2 章 實驗內容與實驗方法

  2.1 引言

  2.2 實驗內容

  2.3 壓電薄膜頂電極制備

  2.4 壓電薄膜性能表征

  2.4.1 相結構表征

  2.4.2 顯微結構表征

  2.4.3 電學性能表征

  2.4.4 高壓拉曼表征

  2.4.5 電子結構表征

  2.5 PMUT 有限元模型的建模與仿真

  2.5.1 有限元方法

  2.5.2 COMSOL 建模仿真流程

  2.5.3 PMUT 三維有限元模型的建立

  2.6 器件結構性能表征

  第 3 章 壓電薄膜的晶體結構與電性能研究

  3.1 引言

  3.2 PZT 薄膜的晶體結構與電學性能

  3.3 Sc0.29Al0.71N 薄膜的晶體結構及其在高壓下的演化

  3.4 本章小結

  第 4 章 基于 PZT 薄膜的 PMUT 建模與性能調控

  4.1 引言

  4.2 基于 PZT 薄膜 PMUT 的建模仿真

  4.3 模態選擇及性能參數評估

  4.4 壓電層對 PMUT 性能的影響

  4.4.1 壓電層厚度對 PMUT 性能的影響

  4.4.2 壓電層面積對 PMUT 性能的影響

  4.4.3 基于不同壓電材料的 PMUT 性能參數對比

  4.5 頂部電極對 PMUT 性能的影響

  4.5.1 電極面積對 PMUT 性能的影響

  4.5.2 電極形狀對 PMUT 性能的影響

  4.5.3 電極材料對 PMUT 性能的影響

  4.6 底部空腔對 PMUT 性能的影響

  4.6.1 底部空腔直徑對 PMUT 性能的影響

  4.6.2 底部空腔形狀對 PMUT 性能的影響

  4.7 襯底頂層硅厚度對 PMUT 性能的影響

  4.8 PMUT 動態特性仿真

  4.9 本章小結

  第 5 章 基于 Sc0.29Al0.71N 薄膜的 PMUT 建模與性能調控

  5.1 引言

  5.2 基于 Sc0.29Al0.71N 薄膜 PMUT 的建模仿真

  5.3 幾何結構對 PMUT 性能的影響

  5.3.1 頂部電極對 PMUT 性能的影響

  5.3.2 底部空腔對 PMUT 性能的影響

  5.3.3 襯底刻蝕深度對 PMUT 性能的影響

  5.4 PMUT 動態特性仿真

  5.5 采用新型壓電材料的 PMUT 模型探索

  目錄 上海師范大學碩士學位論文

  5.6 本章小結

  第 6 章 PMUT 器件制備與性能表征

  6.1 引言

  6.2 PMUT 器件制備

  6.3 器件結構表征

  6.4 位移頻率響應測試

  6.5 脈沖回波測試

  6.6 本章小結

  第 7 章 總結與展望

  7.1 總結

  本論文選取 PMUT 重要壓電材料 PZT 薄膜以及具有高性能的 Sc0.29Al0.71N薄膜展開了晶體結構及電學性能的研究,分別建立了基于這兩種壓電薄膜的高頻PMUT 三維有限元模型,通過探究 PMUT 幾何結構參數對其性能的影響從而實現了性能調控,并制備得到了高頻 PMUT 原型器件。本文的主要結論有:

 。1)以 PZT 薄膜/Pt/Ti/SiO2/Si 和 Sc0.29Al0.71N 薄膜/Mo/SiO2/SOI 為對象對其相結構、顯微結構、電子結構、電學性能等方面進行了研究,結果顯示,PZT薄膜結晶質量良好,其壓電響應明顯,常溫下 1 kHz 時 PZT 薄膜的相對介電常數為 2338,介電損耗僅為 0.027.Sc0.29Al0.71N 薄膜各層分界清晰,表現為六方相多晶薄膜,計算得到其晶格參數 a 和 c 分別為 3.0997 ? 和 4.9569 ?.此外,研究了 Sc0.29Al0.71 薄膜的晶體結構在高壓下的演變行為,在 20 GPa 壓力下并沒有發生纖鋅礦到巖鹽礦的相變,這說明該薄膜的耐高壓特性優良,硬度較高。具有高性能的壓電薄膜為研制高性能壓電微機械超聲換能器的提供了基礎。

 。2)采用有限元分析軟件 COMSOL Multiphysics,分別建立了基于 PZT 薄膜和 Sc0.29Al0.71N 薄膜的高頻 PMUT 三維模型,針對 PMUT(0,1)模態,充分研究了 PMUT 結構中的壓電薄膜厚度和尺寸、頂部電極直徑和形狀、底部空腔直徑和形狀、襯底頂層硅厚度等多種幾何參數對 PMUT 性能的影響,實現了性能調控,其中底部空腔直徑和頂層硅厚度對 PMUT 諧振頻率、靜態靈敏度影響較大。

  此外,研究了水域下 PMUT 模型的動態傳輸接收特性。經過幾何結構優化,基于 PZT 薄膜的 PMUT 模型的諧振頻率可達 22.12 MHz,有效機電耦合系數(????eff2 )為 5.13%,當反射物距離 PMUT 表面中心 300 μm 處時,相對脈沖回波靈敏度級約為-44.7 dB.

 。3)建立了基于 Sc0.29Al0.71N 薄膜的 PMUT 三維有限元模型,經過模型幾何優化,其諧振頻率可達 23.565 MHz,有效機電耦合系數(????eff2 )為 2.5%,當反射物距離 PMUT 表面中心 300 μm 處時,相對脈沖回波靈敏度級約為-50.3 dB.

  此外,還嘗試將沿[011]方向極化的 0.70Pb(Mg1/3Nb2/3)O3-0.30PbTiO3 (PMN-0.30PT)單晶薄膜應用于 PMUT 有限元模型中,探索了在不同頂部電極和底部空腔形狀配置下的 PMUT 模型性能表現。研究發現,這種新型壓電材料以及新型幾何結構為今后實現 PMUT 性能的提升提供了可能。

 。4)依據 PMUT 建模仿真優化得到的幾何結構參數制備了基于 PZT 薄膜PMUT 單元及 50×50 陣列原型器件。PMUT 單元底部空腔刻蝕情況良好,測試第 7 章 總結與展望 上海師范大學碩士學位論文68得到單元器件(0,1)模態下的諧振頻率為 25.87 MHz,回波信號最大幅值為 4.14mV.本論文制備的 PMUT 原型器件滿足了高分辨率超聲成像應用的高頻需求,這為進一步研制出新型高性能 PMUT 器件積累經驗。

  7.2 展望

  鑒于目前已經取得的研究結果,為進一步實現具有高頻高性能的 PMUT,如下工作仍需在此研究基礎上有待開展:

 。1)進一步優化 PMUT 器件制備加工工藝,制備得到基于 Sc0.29Al0.71N 薄膜的高性能 PMUT 單元及陣列原型器件。

 。2)研究具有更高組分的 ScxAl1-xN 壓電薄膜的晶體結構及壓電性能,探究高壓電性能背后的物理機制。

 。3)設計并建立具有新型幾何結構的高性能 PMUT 陣列模型,研究 PMUT陣列模型的旁瓣指數、軸向聲強等頻域發射性能以及聲場特性。

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  致謝

  懷揣對研究生生活的憧憬踏入校園,轉眼間已到畢業離別之季。在此,謹向所有幫助過我與鼓勵過我的各位老師、同學和親友表達衷心的謝意!

  感謝我的導師趙祥永研究員,他學識淵博,治學嚴謹,對科研具有敏銳的洞察力,從本論文工作的選題到最終完成離不開趙老師的悉心指導。趙老師對工作精益求精的態度和為人師表的風范潛移默化地影響著我,除了科研工作上對我的精心教導,趙老師在生活上也予以我無微不至的關心,為我的人生道路點亮明燈,促使我不斷地成長和進步。在此,鄭重地向我的恩師趙老師道一聲感謝!

  感謝上海師范大學的張巧珍老師在我攻讀研究生期間給予的指導、幫助和關心,是張老師帶我走入仿真的大門,她言傳身教,盡職盡責,潛精研思的精神和嚴謹縝密的思維使我深受感染,感謝張老師耐心解答我的每一個問題,反復認真修改我的文章,遇到困難迎難而上的積極態度讓我受益良多,她是良師亦是益友,在此,向張老師道一聲深深的感謝!

  本論文工作的完成離不開各位老師和師兄師姐的指導與幫助。感謝上海師范大學的王飛飛老師、王濤老師、秦曉梅老師、杜偉杰老師、唐艷學老師和段志華老師在科研上對我的幫助。感謝中科院蘇州納米所的李加東老師、苗斌老師以及南京理工大學汪堯進老師在實驗方面給予我的幫助。感謝上海同步輻射光源的郭智老師和閆帥老師在測試方面予以的幫助。感謝姚蒙師兄和郭嘉騏師兄在仿真上給予我無私的指導和幫助,感謝劉旭強師兄在高壓實驗方面提供的幫助。還要感謝上海師范大學的薛賽東師兄、謝青秀師姐、胡鈺晴師姐、周星彤師姐、吳揚師兄、李強師兄以及其他師兄師姐在科研生活中帶給我的幫助和鼓勵。

  衷心感謝研究生期間并肩走過的同學和朋友,感謝我的舍友郭文雨、厙文呈和閆明園,感謝她們的陪伴與鼓勵,優秀的她們是我學習的榜樣。感謝王潔、黃小麗、王巨杉、黎梓浩、鄭群飛、肖俊杰、楊梅和李立新在科研上給予的無私幫助以及給我的研究生生活帶來了無數樂趣。感謝劉會靈師妹、周迅師妹、吳延輝師弟等其他師弟師妹對我的關心與幫助。

  最后,特別感謝我的父母一直以來對我的支持、鼓勵和理解,感謝他們給予我溫馨和睦的家庭氛圍讓我在愛中成長,在此,向我的父母道一聲:辛苦了!還要感謝各位親友對我無條件的支持與鼓勵,正是有了這些愛與支持才使我堅定自信地做自己,我將在未來的道路上繼續勇往直前!

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