氢化硅薄膜介观力学行为研究和耐高温压力传感器研制
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摘要
本文主要针对氢化硅薄膜介观力学行为和耐高温压力传感器这两个问题展开了理论与实验的研究。氢化硅薄膜广泛应用于光电子器件,如二极管、薄膜晶体管、太阳电池、液晶显示器等,人们对其光电特性作了深入的研究,但对力学特性涉及很少。已有的研究表明氢化硅薄膜,尤其是纳米硅薄膜有很强的应力敏感特性,在高灵敏度压力传感器、位移传感器和量子隧道传感器等相关器件应用上有极大的应用前景,因此通过对氢化硅薄膜显微结构与介观力学性能的研究,探明二者之间关系(内禀关联特性)为器件开发的提供基本数据。
本文对射频等离子体增强化学气相沉积(RF-PECVD)系统进行了改造,制备了氢化硅薄膜,成功地进行了磷或硼的掺杂。用拉曼谱揭示了氢化硅薄膜的晶粒平均大小和晶态比;用椭偏仪测试了所制备薄膜的厚度;用X射线衍射谱对薄膜微结构和材料性能的进行了比较。以相同的工艺在玻璃和单晶硅衬底上制备了本征或掺磷(硼)的纳米硅薄膜,对不同衬底上纳米硅薄膜进行了对比研究,发现衬底对薄膜生长速率影响不大,但所制备薄膜的微观结构有很大的差异。相同工艺条件下,在玻璃衬底上生长的薄膜,表面粗糙度小于单晶硅衬底上的薄膜;而晶化程度低于单晶硅衬底。掺杂使微结构有了变化,掺磷促进晶化,掺硼促进非晶化。
用不同波长的激光线对单晶硅,纳米硅薄膜和非晶硅薄膜拉曼散射实验,发现拉曼线形随激光线波长的不同而不同。当用紫外光短波长325nm激光线激发时,由于穿透深度浅,在318.2cm~(-1)处出现了小峰。无论单晶硅衬底还是玻璃衬底的硅薄膜,当用785nm激光线激发时,由于穿透深度深,对单晶硅衬底的薄膜,反映了衬底的信息,在520.0cm~(-1)附近有尖锐的谱峰;而对玻璃衬底的薄膜而言,则是弥散的拉曼光谱,反应了玻璃衬底非晶无序的微结构特征。对氢化硅薄膜介观力学行为及其与微结构内禀关联特性进行了研究,发现相同的晶态比,制备于玻璃衬底上的氢化硅薄膜由于存在非晶态的过渡缓冲层,弹性模量小于相应的制备于单晶硅衬底上的氢化硅薄膜。由于磷的掺入,薄膜中晶粒细化,有序度提高,薄膜的晶态比一般在40%以上。硼的掺入,晶态比减小,一般低于40%。同时发现对掺磷,本征和掺硼的氢化硅薄膜,分别在晶态比为45%,30%和15%左右,弹性模量最小。这些研究结果对器件级硅薄膜的制备以及器件化有重要的指导意义。
针对高灵敏度纳米硅薄膜压力传感器的研究,本文进行了耐高温压力传感器的研究。传统的硅扩散压阻式压力传感器用重掺杂4个p型硅应变电阻构成惠斯顿电桥的力敏检测模式,采用pn结隔离,当温度在100℃以上时,pn结漏电流很大,使器件无法工作。制作耐高温压阻式压力传感器,必须取消pn结隔离,较易的方法之一是采用绝缘体介质隔离(silicon on insulator,SOI)结构。本文研究了单晶硅的晶面和晶向的特性,结合硅微加工工艺,针对高温高压的要求,采用圆平膜芯片,以单晶硅(100)晶面为工作面,两对桥臂力敏电阻分别布置在互相垂直的[110]和[1(?)0]晶向上,位于圆膜边缘处,从而获得了四个臂的差动等臂等应变的惠斯登检测电桥。采用SIMOX技术,在n型硅片上高能注入氧离子,获得了优质商用的SOI晶片,在微加工平台上,制作了耐高温压力传感器芯片,尺寸为5.0mm×5.0mm×0.5mm。制作了硅芯片/玻璃环静电键合装置,完成了硅芯片/玻璃环静电键合。制作了热压焊工作台,选用退火后的金丝,通过金金连接完成内引线键合。掌握了耐高温胶粘剂的实用配比及固化工艺;自制了耐高温覆铜传引板,采用含银的高温焊锡丝,选用耐高温导线作为外导线,完成了耐高温传感器封装的关键部分。
选用恒流源激励,设计了温度补偿电路,用对温度求导数的数学方法,推导了灵敏度热漂移(temperature coefficient of sensitivity,TCS)、热零点漂移(temperature coefficient of offset,TCO)和零位输出(offsetshift of voltage,V_(os))漂移补偿计算公式,实现了宽温区温度系数补偿,在-20℃～200℃补偿温区内,通过温度循环标定,经补偿后TCS和TCO的值均小于1.0×10~(-4)/℃·FS;非线性误差小于0.1%FS,不重复性和迟滞误差均小于0.05%FS,总精度小于0.2%FS,高、低温时漂均小于0.1mV/8h,获得了量程从0～40MPa、耐温-40～220℃,具有一定抗瞬时高温冲击能力,高精度稳定性佳的压阻式压力传感器,静态技术指标优于同类型Kulite公司产品。后又用针对适用于塑料、橡胶、化纤、蒸汽、热油等高温介质压力的测量工况,采用分体结构,研制了通用型分体式耐高温压力传感器,用汞作为传压介质,使被测高温高压液体或气体与敏感元件隔离开来,大大地拓宽了工作温区,使传感器工作温度提高到350℃。
This thesis gives an overview of mesoscopic mechanical behavior of hydrogenated silicon thin film and high pressure sensor fabricaton.Hydrogenated silicon thin films have been widely used in electronic and optoelectronic devices such as diodes,thin film transistors,solar cells,liquid crystal display.The research up to date has mainly been concentrated on the film electrical and optical properties and much less on the mechanical ones.However hydrogenated silicon thin films have received great attention due to their sensitive response under mechanical strain and pursued because of its potential advantages for fabrication of high sensitivity piezoresistive pressure sensors, displacement sensors and integrated tunneling sensors.So it is important to understand the mesoscopic mechanical characterization of hydrogenated silicon thin films and the intrinsic relationship with the microstructure.
Hydrogenated silicon films were deposited on glass and single crystalline silicon substrate in a capacitive coupled radio-frequent(RF of 13.56MHz) PECVD system aided with direct current(dc) bias stimulation.The thickness of the thin films is measured using spectroscopic ellipsometry measuring system.X-ray diffraction was used to characterize the structure of the silicon films and grain size determination. Raman spectroscopy was performed to verify the crystalline structure and to determine the structural composition of the silicon films.Atomic force microscopy was used to investigate the topography and roughness of the films.It is shown little difference of film thickness exists and deposition rate is little affected with different substrates while microstructure of the thin films varies with different substrate.Under the same deposition condition,the films on single crystalline silicon provide better crystallinty than that on glass substrate while they have much smaller rms roughness than that deposited on single crystalline silicon.It means that the silicon atoms on glass surface have no significant diffusion.They essentially condense wherever they land on the surface of the substrate.It is also suggested that the chemical nature of the substrate surface influences the initial stage of the growth.
Nanocrystalline silicon and amorphous silicon thin films are grown on the single crystalline silicon and glass substrate,respectively.Raman scattering is used on those films by three different excitation wavelengths,from red to near ultraviolet.It is found that the Raman spectrometry is different by varying the incident wavelength.We probe the incident light intensity energy,the photo absorption coefficient of silicon respectively and the Penetration depth.The experiment result is well explained and it is shown that to get further information of material microstructure optimum laser should be chosen.Mesoscopic mechanical characterization of hydrogenated silicon film is gotten by nanoindentation based on the conventional depth-sensing indentation method. The crystalline volume fraction(X_c) is obtained from the Raman spectra.An analytical relation between Xc and elastic modulus is established.It is shown the elastic modulus of the film on glass substrate is lower than that on silicon with the same Xc.The grain size of phosphorus doping thin film is smaller than that of intrinsic one and more ordered.The Xc is usually above 40%.The film with diborane doping is on the appetite side.The Xc is usually below 40%.To P-doped,intrinsic and B-doped fims,when Xc is 45%,30%and 15%respectively,the elastic modulus are lower.These results should have important impacts on the engineering of nanocrystalline silicon and related devices.
There is a growing requirement for piezoresistive pressure sensor to operate in high temperature and harsh environment.Typical such areas are in the oil industry and a host of others.The conventional piezoresistive pressure sensors are made by forming diffused or ion implanted strain gauges in a Wheatstone bridge configuration on the thin silicon diaphragm.A known limitation of these silicon-based devices using isolation by reverse biased pn-junctions is the rising junction leakage current at elevated temperatures up to 100℃,which make them in unstable state.One of the promising attempts for fabrication of high temperature piezoresistive pressure sensors is to cancel pn-insulation of the piezoresistors.We use the separation by implanted oxygen(SIMOX) method,which is one of the two mainstream methods supplying commercial silicon-on-insulator(SOI) wafers,to design and fabricate the sensing chip dielectrically insulated by SiO_2.For the purposes of pressure measurement for low cost high temperature application,the mechanical structure is designed for operation between the temperature of—40～220℃and the range of 0～40MPa.Using high temperature packaging process and excitation of constant current,the sensor is testified with precise accuracy and stability.The specific works finished and main innovative contributions of this dissertation are as follows.
The characteristic of silicon plane and direction is researched with micro machining and anisotropic-etching technology.For the requirement of operation in high temperature and high pressure,we choose the design of circular plane membrane.In the structure,two pairs of the strain gauges of the Wheatstone bridge are placed respectively on the direction[110]and[110]which are perpendicular each other on the (100) plane of the surface silicon layer.Four strain gauges are on the fringe of the diaphragm.Two gauges are along the direction of[110]while the other two are perpendicular to the direction of[110].For these four gauges they are parallel each other to make the Wheatstone detective bridge of four equal strains and resistances. Using SIMOX process a large dose of oxygen is implanted into the silicon wafer.The beam energy is 200keV with 1.8×10~(18)O~+/cm~2 and the target substrate is kept at 650℃to get high-quality SOI wafer.Furthermore,the sensor chip of wide range is fabricated in micro machining work bay.The size of it is 5.0mm×5.0mm×0.5mm.
The electrostatic bonding of silicon and Prex7740 glass ring is done on self-made experimental instrument.The gold wire thermocompression bonding worktable is also made for wire bonding.The board covered with Cu is fabricated for leading.The soldering tin thread and lead wire is required for high temperature operation.Using high temperature packaging process,the sensor is testified with precise accuracy and excellent stability and reliability.
The temperature coefficient of sensitivity(TCS) and temperature coefficient of offset(TCO) compensation circuit is selected and easily done in using a constant current of 2mA.A quantitative compensation formula is introduced in mathematics by the derivative of the equation above with respect to temperature.Using this circuit and result,the absolute value of the sensor's TCS and TCO is easy to be less than 100×10 ~6/℃.FSO by calibration of several temperature compensation cycles.Most non-linearity and hysteresis of the sensors are less than 0.1%FSO and 0.05%FSO,respectively.The sensitivity at the temperature of 220℃is 0.37～0.8mV/V/MPa due to different chips. Since the micro machining process methodology has been consistently proved to be reproducible,its batch production offers the advantage of low cost,reduced process time,and high yield.Thanks to high temperature packaging,the characteristics of the sensor are shown to be satisfied when operating at high temperature.
This work is supported by "Six top talent" project of Jiangsu Province(Grant No. 06-D-022),National Basic Research Program of China(Grant No.2004CB619305),the technology development plan of Zhejiang Province(Grant No.2005C31048),doctoral innovation plan of Jiangsu University and the fifth undergraduate scientific research project of Jiangsu University(Grant No.05A036).
本文对射频等离子体增强化学气相沉积(RF-PECVD)系统进行了改造,制备了氢化硅薄膜,成功地进行了磷或硼的掺杂。用拉曼谱揭示了氢化硅薄膜的晶粒平均大小和晶态比;用椭偏仪测试了所制备薄膜的厚度;用X射线衍射谱对薄膜微结构和材料性能的进行了比较。以相同的工艺在玻璃和单晶硅衬底上制备了本征或掺磷(硼)的纳米硅薄膜,对不同衬底上纳米硅薄膜进行了对比研究,发现衬底对薄膜生长速率影响不大,但所制备薄膜的微观结构有很大的差异。相同工艺条件下,在玻璃衬底上生长的薄膜,表面粗糙度小于单晶硅衬底上的薄膜;而晶化程度低于单晶硅衬底。掺杂使微结构有了变化,掺磷促进晶化,掺硼促进非晶化。
用不同波长的激光线对单晶硅,纳米硅薄膜和非晶硅薄膜拉曼散射实验,发现拉曼线形随激光线波长的不同而不同。当用紫外光短波长325nm激光线激发时,由于穿透深度浅,在318.2cm~(-1)处出现了小峰。无论单晶硅衬底还是玻璃衬底的硅薄膜,当用785nm激光线激发时,由于穿透深度深,对单晶硅衬底的薄膜,反映了衬底的信息,在520.0cm~(-1)附近有尖锐的谱峰;而对玻璃衬底的薄膜而言,则是弥散的拉曼光谱,反应了玻璃衬底非晶无序的微结构特征。对氢化硅薄膜介观力学行为及其与微结构内禀关联特性进行了研究,发现相同的晶态比,制备于玻璃衬底上的氢化硅薄膜由于存在非晶态的过渡缓冲层,弹性模量小于相应的制备于单晶硅衬底上的氢化硅薄膜。由于磷的掺入,薄膜中晶粒细化,有序度提高,薄膜的晶态比一般在40%以上。硼的掺入,晶态比减小,一般低于40%。同时发现对掺磷,本征和掺硼的氢化硅薄膜,分别在晶态比为45%,30%和15%左右,弹性模量最小。这些研究结果对器件级硅薄膜的制备以及器件化有重要的指导意义。
针对高灵敏度纳米硅薄膜压力传感器的研究,本文进行了耐高温压力传感器的研究。传统的硅扩散压阻式压力传感器用重掺杂4个p型硅应变电阻构成惠斯顿电桥的力敏检测模式,采用pn结隔离,当温度在100℃以上时,pn结漏电流很大,使器件无法工作。制作耐高温压阻式压力传感器,必须取消pn结隔离,较易的方法之一是采用绝缘体介质隔离(silicon on insulator,SOI)结构。本文研究了单晶硅的晶面和晶向的特性,结合硅微加工工艺,针对高温高压的要求,采用圆平膜芯片,以单晶硅(100)晶面为工作面,两对桥臂力敏电阻分别布置在互相垂直的[110]和[1(?)0]晶向上,位于圆膜边缘处,从而获得了四个臂的差动等臂等应变的惠斯登检测电桥。采用SIMOX技术,在n型硅片上高能注入氧离子,获得了优质商用的SOI晶片,在微加工平台上,制作了耐高温压力传感器芯片,尺寸为5.0mm×5.0mm×0.5mm。制作了硅芯片/玻璃环静电键合装置,完成了硅芯片/玻璃环静电键合。制作了热压焊工作台,选用退火后的金丝,通过金金连接完成内引线键合。掌握了耐高温胶粘剂的实用配比及固化工艺;自制了耐高温覆铜传引板,采用含银的高温焊锡丝,选用耐高温导线作为外导线,完成了耐高温传感器封装的关键部分。
选用恒流源激励,设计了温度补偿电路,用对温度求导数的数学方法,推导了灵敏度热漂移(temperature coefficient of sensitivity,TCS)、热零点漂移(temperature coefficient of offset,TCO)和零位输出(offsetshift of voltage,V_(os))漂移补偿计算公式,实现了宽温区温度系数补偿,在-20℃～200℃补偿温区内,通过温度循环标定,经补偿后TCS和TCO的值均小于1.0×10~(-4)/℃·FS;非线性误差小于0.1%FS,不重复性和迟滞误差均小于0.05%FS,总精度小于0.2%FS,高、低温时漂均小于0.1mV/8h,获得了量程从0～40MPa、耐温-40～220℃,具有一定抗瞬时高温冲击能力,高精度稳定性佳的压阻式压力传感器,静态技术指标优于同类型Kulite公司产品。后又用针对适用于塑料、橡胶、化纤、蒸汽、热油等高温介质压力的测量工况,采用分体结构,研制了通用型分体式耐高温压力传感器,用汞作为传压介质,使被测高温高压液体或气体与敏感元件隔离开来,大大地拓宽了工作温区,使传感器工作温度提高到350℃。
This thesis gives an overview of mesoscopic mechanical behavior of hydrogenated silicon thin film and high pressure sensor fabricaton.Hydrogenated silicon thin films have been widely used in electronic and optoelectronic devices such as diodes,thin film transistors,solar cells,liquid crystal display.The research up to date has mainly been concentrated on the film electrical and optical properties and much less on the mechanical ones.However hydrogenated silicon thin films have received great attention due to their sensitive response under mechanical strain and pursued because of its potential advantages for fabrication of high sensitivity piezoresistive pressure sensors, displacement sensors and integrated tunneling sensors.So it is important to understand the mesoscopic mechanical characterization of hydrogenated silicon thin films and the intrinsic relationship with the microstructure.
Hydrogenated silicon films were deposited on glass and single crystalline silicon substrate in a capacitive coupled radio-frequent(RF of 13.56MHz) PECVD system aided with direct current(dc) bias stimulation.The thickness of the thin films is measured using spectroscopic ellipsometry measuring system.X-ray diffraction was used to characterize the structure of the silicon films and grain size determination. Raman spectroscopy was performed to verify the crystalline structure and to determine the structural composition of the silicon films.Atomic force microscopy was used to investigate the topography and roughness of the films.It is shown little difference of film thickness exists and deposition rate is little affected with different substrates while microstructure of the thin films varies with different substrate.Under the same deposition condition,the films on single crystalline silicon provide better crystallinty than that on glass substrate while they have much smaller rms roughness than that deposited on single crystalline silicon.It means that the silicon atoms on glass surface have no significant diffusion.They essentially condense wherever they land on the surface of the substrate.It is also suggested that the chemical nature of the substrate surface influences the initial stage of the growth.
Nanocrystalline silicon and amorphous silicon thin films are grown on the single crystalline silicon and glass substrate,respectively.Raman scattering is used on those films by three different excitation wavelengths,from red to near ultraviolet.It is found that the Raman spectrometry is different by varying the incident wavelength.We probe the incident light intensity energy,the photo absorption coefficient of silicon respectively and the Penetration depth.The experiment result is well explained and it is shown that to get further information of material microstructure optimum laser should be chosen.Mesoscopic mechanical characterization of hydrogenated silicon film is gotten by nanoindentation based on the conventional depth-sensing indentation method. The crystalline volume fraction(X_c) is obtained from the Raman spectra.An analytical relation between Xc and elastic modulus is established.It is shown the elastic modulus of the film on glass substrate is lower than that on silicon with the same Xc.The grain size of phosphorus doping thin film is smaller than that of intrinsic one and more ordered.The Xc is usually above 40%.The film with diborane doping is on the appetite side.The Xc is usually below 40%.To P-doped,intrinsic and B-doped fims,when Xc is 45%,30%and 15%respectively,the elastic modulus are lower.These results should have important impacts on the engineering of nanocrystalline silicon and related devices.
There is a growing requirement for piezoresistive pressure sensor to operate in high temperature and harsh environment.Typical such areas are in the oil industry and a host of others.The conventional piezoresistive pressure sensors are made by forming diffused or ion implanted strain gauges in a Wheatstone bridge configuration on the thin silicon diaphragm.A known limitation of these silicon-based devices using isolation by reverse biased pn-junctions is the rising junction leakage current at elevated temperatures up to 100℃,which make them in unstable state.One of the promising attempts for fabrication of high temperature piezoresistive pressure sensors is to cancel pn-insulation of the piezoresistors.We use the separation by implanted oxygen(SIMOX) method,which is one of the two mainstream methods supplying commercial silicon-on-insulator(SOI) wafers,to design and fabricate the sensing chip dielectrically insulated by SiO_2.For the purposes of pressure measurement for low cost high temperature application,the mechanical structure is designed for operation between the temperature of—40～220℃and the range of 0～40MPa.Using high temperature packaging process and excitation of constant current,the sensor is testified with precise accuracy and stability.The specific works finished and main innovative contributions of this dissertation are as follows.
The characteristic of silicon plane and direction is researched with micro machining and anisotropic-etching technology.For the requirement of operation in high temperature and high pressure,we choose the design of circular plane membrane.In the structure,two pairs of the strain gauges of the Wheatstone bridge are placed respectively on the direction[110]and[110]which are perpendicular each other on the (100) plane of the surface silicon layer.Four strain gauges are on the fringe of the diaphragm.Two gauges are along the direction of[110]while the other two are perpendicular to the direction of[110].For these four gauges they are parallel each other to make the Wheatstone detective bridge of four equal strains and resistances. Using SIMOX process a large dose of oxygen is implanted into the silicon wafer.The beam energy is 200keV with 1.8×10~(18)O~+/cm~2 and the target substrate is kept at 650℃to get high-quality SOI wafer.Furthermore,the sensor chip of wide range is fabricated in micro machining work bay.The size of it is 5.0mm×5.0mm×0.5mm.
The electrostatic bonding of silicon and Prex7740 glass ring is done on self-made experimental instrument.The gold wire thermocompression bonding worktable is also made for wire bonding.The board covered with Cu is fabricated for leading.The soldering tin thread and lead wire is required for high temperature operation.Using high temperature packaging process,the sensor is testified with precise accuracy and excellent stability and reliability.
The temperature coefficient of sensitivity(TCS) and temperature coefficient of offset(TCO) compensation circuit is selected and easily done in using a constant current of 2mA.A quantitative compensation formula is introduced in mathematics by the derivative of the equation above with respect to temperature.Using this circuit and result,the absolute value of the sensor's TCS and TCO is easy to be less than 100×10 ~6/℃.FSO by calibration of several temperature compensation cycles.Most non-linearity and hysteresis of the sensors are less than 0.1%FSO and 0.05%FSO,respectively.The sensitivity at the temperature of 220℃is 0.37～0.8mV/V/MPa due to different chips. Since the micro machining process methodology has been consistently proved to be reproducible,its batch production offers the advantage of low cost,reduced process time,and high yield.Thanks to high temperature packaging,the characteristics of the sensor are shown to be satisfied when operating at high temperature.
This work is supported by "Six top talent" project of Jiangsu Province(Grant No. 06-D-022),National Basic Research Program of China(Grant No.2004CB619305),the technology development plan of Zhejiang Province(Grant No.2005C31048),doctoral innovation plan of Jiangsu University and the fifth undergraduate scientific research project of Jiangsu University(Grant No.05A036).
引文
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