WO2017080340A1 - Dispositif de mesure de propriété piézorésistive géante de nanofil et son procédé de fabrication - Google Patents

Dispositif de mesure de propriété piézorésistive géante de nanofil et son procédé de fabrication Download PDF

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WO2017080340A1
WO2017080340A1 PCT/CN2016/102073 CN2016102073W WO2017080340A1 WO 2017080340 A1 WO2017080340 A1 WO 2017080340A1 CN 2016102073 W CN2016102073 W CN 2016102073W WO 2017080340 A1 WO2017080340 A1 WO 2017080340A1
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nanowire
silicon
nanowires
etching
oxide layer
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PCT/CN2016/102073
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Chinese (zh)
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张加宏
赵阳
李敏
杨敏
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南京信息工程大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R3/00—Apparatus or processes specially adapted for the manufacture or maintenance of measuring instruments, e.g. of probe tips

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  • the invention relates to a nanowire giant piezoresistive characteristic measuring device and a manufacturing method thereof, and belongs to the technical field of micro-nano electromechanical systems.
  • nanowires As a typical one-dimensional semiconductor nanomaterial, nanowires have the characteristics of general nanomaterials, compatibility with modern large-scale integrated circuit technology, easy preparation in large quantities, and easy surface modification. Because the semiconductor properties of nanowires show unique electrical, mechanical, thermal, and chemical properties, their research and application areas cover a wide range of fields from chemical, physical, biological, environmental sensors, field effect transistors, and logic circuits. In addition, silicon nanowires also exhibit field emission, thermal conductivity, visible light luminescence and quantum confinement effects different from bulk silicon materials, and have great potential applications in nanoelectronic devices, optoelectronic devices and new energy sources. .
  • the giant piezoresistive effect has become the most interesting feature due to its potential use in electromechanical sensors and strain engineering.
  • the preparation methods are as follows: 1. Reducing the diameter of the nanowires by repeated thermal oxidation and etching processes to form a significant quantum confinement effect to enhance the nanometers.
  • the piezoresistive characteristics of the wire 2. Surface modification of the nanowire by a chemical process; 3. Preparation of a semiconductor-metal heterostructure.
  • the current characterization of nanostructured piezoresistive coefficients can be divided into two main categories: one is based on Atomic Force Microscope (AFM) or other probe technology loading methods, the main feature is the need for AFM/ Probe integrated nanomechanical sensor and nano
  • the meter precision actuator requires nano-manipulation technology to assemble the nanostructure onto the needle tip and so on.
  • AFM Atomic Force Microscope
  • Such experimental test systems are very complicated and the experimental costs are also very expensive.
  • the size of the AFM tip structure is much larger than that of the nanostructure, and the control accuracy during mechanical loading is difficult to reach the nanometer scale.
  • most AFM mechanical loading experiments are performed in Scanning Electron Microscopy (SEM), which affects the measurement of electrical characteristics.
  • the other is to use the micro-electro-mechanical system micro-actuator to load the nano-structure.
  • MEMS driving devices piezoelectric driving, electrostatic comb driving and thermal driving.
  • the measurement of the resistance is measured by two points. The existence of factors such as resistance undoubtedly increases the measurement error of the piezoresistive coefficient of the nanowire.
  • the present invention provides a nanowire giant piezoresistive characteristic measuring device and a manufacturing method thereof.
  • a nanowire giant piezoresistive characteristic measuring device comprises: a nanowire, a platinum resistance temperature sensor, an electrothermal actuator, a displacement sensor based on capacitance measurement, an electrode, a load sensor based on capacitance measurement, the platinum resistance temperature sensor, and an electric heating
  • An actuator, a displacement sensor based on capacitance measurement, and a load sensor based on capacitance measurement are sequentially connected, and the number of electrodes is set to four, the four The electrodes are disposed between the displacement sensor based on the capacitance measurement and the load sensor based on the capacitance measurement, and nanowires are disposed between the two horizontally placed electrodes, and electrodes are disposed on the lower sides of the nanowires.
  • a calibration probe that is coupled to a load sensor based on capacitance measurements.
  • the invention further comprises an electrical insulation module, characterized in that: between the electrothermal actuator and the displacement sensor based on the capacitance measurement, between the displacement sensor and the electrode based on the capacitance measurement, and between the electrode and the load sensor based on the capacitance measurement, based on the capacitance An electrical insulation module is provided between the measured load cell and the calibration probe.
  • the nanowires are made of externally grown silicon nanowires, and surface-modified by silver nanoparticles prepared on the nanowires to form a giant piezoresistive property.
  • the nanowires are chemical vapor deposition methods for synthesizing silicon germanium radial heterostructure nanowires having giant piezoresistive properties based on radial and axial growth control.
  • the nanowires are self-assembled by solution meteorological method to self-assemble silicon germanium longitudinal heterojunction nanowires having giant piezoresistive properties.
  • the nanowire adopts STM tip operation to prepare the nanowire with giant piezoresistive characteristics to position, align, and tighten the nanowires on the upper surface of the two suspension electrodes, and use the electron beam to induce deposition of the nanowires.
  • the array is attached to the suspension electrode.
  • a method for manufacturing a nanowire giant piezoresistive characteristic measuring device comprising: the following steps:
  • Step 1 Select 25 ⁇ m of top silicon, bury 2 ⁇ m of oxide layer, and 300 ⁇ m of SOI silicon wafer of bottom silicon.
  • the silicon wafer is placed in a mixed solution of acetone, hydrogen peroxide and concentrated sulfuric acid for ultrasonic cleaning, and then repeatedly cleaned with deionized water. Then, the cleaned silicon wafer is placed in a diluted HF solution to remove the oxide layer on the surface of the silicon wafer;
  • Step 2 depositing a 1 ⁇ m SiO 2 oxide layer on the top layer and the bottom layer of the SOI wafer by LPCVD technology;
  • Step Three forming a platinum resistance region is etched by RIE technique SiO 2 top oxide layer; etching by DRIE technique platinum resistance region;
  • Step 4 etching the top SiO 2 oxide layer by RIE technique to form a boron doped resistance region; boron doping is performed in the resistance region by a diffusion process, and the resistivity of the resistive region is set to 1.7 to 1.9 ⁇ 10 ⁇ 5 ⁇ ⁇ m, forming a P-type doped silicon resistance region;
  • Step 5 etching the SiO 2 oxide layer on the silicon surface by BOE using a buffer oxide
  • Step 6 etching the underlying SiO 2 oxide layer by an RIE technique to form an insulating module pattern
  • Step 7 spin-coating a photoresist on the bottom layer of the SOI silicon wafer; forming a oxide layer etching mask pattern by using a mask;
  • Step 8 etching the underlying silicon by 100 ⁇ m by DRIE technology
  • Step 9 etching the underlying SiO 2 oxide layer not protected by the photoresist by an RIE technique
  • Step 10 etching the underlying silicon not protected by the photoresist and the oxide layer by DRIE technology
  • Step 11 forming a platinum resistive pattern using a positive photoresist, and using a stripping process to form a platinum unit of a temperature unit on the SiO 2 buried layer;
  • Step 12 forming a pattern of electrodes and lead regions using a positive photoresist; sputtering aluminum, using a stripping process to form leads and an aluminum upper electrode;
  • Step 13 etching the SiO2 buried layer by RIE technology to expose the insulating module
  • Step 14 stripping the residual photoresist, the underlying SiO 2 oxide layer
  • Step 15 The device structure is completed by DRIE technology on the top layer silicon to form a complete structure and then annealed, and the aluminum lower electrode is formed on the measurement substrate by photolithography, etching, and stripping processes.
  • the nanowire giant piezoresistive characteristic measuring device and the manufacturing method thereof provided by the present invention use a combination of an external electric field and a chemical process surface modification to modify the surface state structure of the nanowire, or use self-grown silicon.
  • the heterostructure is used to complete the preparation of nanowires with giant piezoresistive properties.
  • the nanowire giant piezoresistive characteristic measuring device is completed by using a standard CMOS process compatible MEMS technology suitable for mass production, and the MEMS measuring device can simultaneously measure the mechanical characteristics and electrical characteristics of the nanowire, thereby completing the characterization of the piezoresistive coefficient. And can be applied to a variety of different measurement samples.
  • the measuring device obtains the elongation and load data of the nanowire through the capacitance digital conversion chip which is externally connected to the displacement sensor and the load sensor, and thus does not depend on the scanning electron microscope imaging, thereby avoiding the measurement of the electrical characteristics by the electron beam irradiation. influences.
  • the measuring device also integrates a temperature sensor for temperature compensation of the piezoresistive coefficient, reducing the influence of the environmental system, thereby completing the high piezoresistive coefficient of various measurement samples. The purpose of precision measurement.
  • the present invention provides a method for preparing five kinds of nanowires having giant piezoresistive characteristics, and the MEMS measuring device with giant piezoresistive characteristics has the ability to apply a bias electric field, and can modulate the piezoresistive characteristics of the nanowires.
  • the invention integrates the MEMS temperature sensor with the measuring device for temperature compensation, ensures the consistency, and improves the accuracy of the giant piezoresistive coefficient.
  • the present invention combines the four-probe structure to eliminate the influence of contact resistance and thereby make the measurement result of the nanowire giant piezoresistive coefficient more accurate.
  • the present invention provides a higher sampling rate that can be captured in emergent events such as plastic deformation and corrupted data points.
  • the apparatus of the present invention can be characterized outside the vacuum chamber to make it easier to study the effects of environmental factors on the properties of the nanomaterial, such as gas, light or temperature.
  • the measurement sample of the present invention may be a two-dimensional film, a one-dimensional nanostructure, and the nanostructure may be a single semiconductor nanowire structure, which may be a heterojunction nanowire or a nanowire array.
  • FIG. 1 is a schematic structural view of a nanowire giant piezoresistive characteristic measuring device
  • FIG. 2 is a working flow chart of a nanowire giant piezoresistive characteristic measuring device
  • FIG. 3 is a flow chart of a preparation process of a nanowire giant piezoresistive characteristic measuring device
  • FIG. 4 is a schematic view showing the preparation of a silicon germanium radial heterojunction nanowire
  • FIG. 5 is a schematic view showing growth of a silicon germanium longitudinal heterojunction nanowire
  • Figure 6 is a schematic view showing the operation of the STM probe to fix the nanowires on the electrodes
  • FIG. 7 is a schematic view of nanowires self-growth on an electrode
  • FIG. 8 is a flow chart of a MEMS process prepared by an integrated measurement structure of an electron beam lithography nanowire;
  • FIG. 9 is a schematic structural view of four electrodes of a nanowire
  • Figure 10 is a mechanical model of a mechanical characterization device for a nanowire sample
  • Figure 11 is a flow chart of temperature compensation for wavelet neural network based on improved genetic algorithm.
  • a nanowire giant piezoresistive characteristic measuring device is a platinum resistance temperature sensor 1 for temperature compensation from left to right, and an electrothermal actuator 2 for driving a displacement sensor and a nanowire. And load sensor movement; displacement sensor 3 based on capacitance measurement for measuring the displacement of the thermal actuator while achieving the drive voltage decoupling function of the thermal actuator; four electrodes 4 for four-probe measurement; Nanowire 6 with giant piezoresistive characteristics; load sensor 9 based on capacitance measurement for measuring the displacement and tension of itself; calibration probe 10 for calibrating the force sensor. All of the above units are stabilized in the same plane by a set of beams anchored to the top silicon to ensure uniform distribution of the entire nanowire specimen.
  • the electrothermal actuator 2 and the displacement sensor 3, the displacement sensor 3 and the electrode 4, the electrode 4 and the load sensor 9, the load sensor 9 and the calibration probe 10 are respectively mechanically connected through the electrically insulating modules 11 of the four SOI buried layers, Independent electrical measurements are provided for nanowire samples; also used for mechanical connection of load sensor 9 to calibration probe 10 for efficient measurement.
  • the two suspension electrodes 4 are mechanically connected to the nanowires 6.
  • a measuring step of a nanowire giant piezoresistive characteristic measuring device in the first step, the displacement sensor and the load sensor are calibrated under a microscope; and in the second step, the electrothermal actuator is driven as a driving device through an insulation module.
  • the displacement sensor moves to the left, and the nanowire is moved to the left by the insulation module, and the nanowire is also moved to the left by the insulation module;
  • the third step is the capacitance digital conversion by the load sensor and the displacement sensor based on the capacitance measurement
  • the chip obtains the load and elongation data of the nanowire, and at the same time, the piezoresistive change is obtained by the measurement of the four probes; in the fourth step, the piezoresistive effect is characterized by the strain coefficient.
  • the device structure is completed by DRIE technology on the top layer silicon to form a complete structure and then annealed, and the aluminum lower electrode is formed on the measurement substrate by photolithography, etching and stripping processes.
  • the calibration of the load sensor and the displacement sensor is completed.
  • the data sampling rate for device calibration is 45 Hz.
  • the displacement sensor and the electrothermal actuator are moved to the left, and the displacement of the displacement sensor in the microscopic imaging and the displacement of the capacitance digital conversion chip circuit corresponding to the displacement are read out.
  • the voltage is output, and the relationship between the displacement sensors and the corresponding voltage outputs is obtained.
  • the probe device is used to push the calibration probe to move, and the displacement of the load sensor in the microscopic imaging and the output voltage of the capacitance digital conversion chip circuit corresponding to the displacement are read out, and the relationship between the load sensor and the corresponding voltage output is obtained.
  • the load cell is calibrated using a precision microbalance to obtain the relationship between displacement and load.
  • the invention provides five nanowire setting methods with giant piezoresistive characteristics, as follows:
  • Example 1 Silicon nanowires with silver
  • the oxide film on the nanowire is treated with hydrofluoric acid, the surface of the nanowire of silicon is passivated by hydrogen, and the silicon nanoparticle whose surface is passivated by hydrogen is put into the silver nitrate solution, and the nanometer of silver is prepared on the silicon nanowire. particle.
  • Example 2 Silicon germanium radial heterojunction nanowires
  • Gold nanoclusters are deposited on oxidized silicon wafers and placed in a quartz tube furnace.
  • silane was used as the lead gas, so that the silicon nanowire core was grown at an axial growth rate of about 2 ⁇ m/min, and then p-type silicon shell was deposited using silane and 100 ppm helium diborane as a lead gas. And at a radial growth rate of 10 nm/min.
  • ⁇ nanowire 10% The relevant argon gas was grown at an axial growth rate of 0.72 um/min, and the crucible was deposited in the furnace at a radial velocity of 10 nm/min by changing the positional environment of the growth substrate.
  • Nanowires of various core-shell structures such as Si/Ge, Ge/Si, or Si/Ge/Si, Ge/Si/Ge, etc., can be completed by repeating the above process.
  • the process flow chart is shown in Figure 4.
  • a clean silicon wafer washed with an organic solvent is placed in a vacuum sputtering coating machine, and a layer of about 10 nm of tin is sputtered on the surface of the silicon wafer, heated to 600 ° C, and tin is agglomerated into nanoparticles;
  • silane gas is obtained by thermal decomposition of wrong silane, and then silane gas is used as a lead gas to grow silicon nano-fragments on the surface of the tin nano-particle catalyst layer, and the reaction is completed and then (Ar + 5% H 2 ) gas is introduced.
  • the residual precursor gas is removed; in the third step, the triphenyl decane liquid is thermally decomposed at 420-440 ° C to obtain a decane gas, which is then used as a lead gas for growing the yttrium nano-segment on the silicon nano-fragment.
  • the ruthenium nano-fragment was grown, and after completion of the reaction, an (Ar + 5% H 2 ) gas was introduced to remove residual residual precursor gases.
  • the silicon germanium heterojunction nanowires of the abrupt interface are formed by repeating the above two steps repeatedly, and the structure is until a suitable length of silicon germanium heterojunction nanowires (Si/Ge/Si/Ge) is grown.
  • the process flow chart is shown in Figure 5.
  • the STM (sweep-to-tunnel microscope) tip operation was used to position, align, and tighten the nanowires on the upper surfaces of the two suspension electrodes, and the electron beam induced deposition.
  • the nanowire array is fixed to the suspension electrode, and the effect is shown in Fig. 6.
  • a thin oxide layer of 30-60 nm is formed on the model, and then lithographically positioned to remove oxidation of the sidewall of the trench
  • the layer forms a window for growing silicon nanowires.
  • Photolithography is used to assist in locating the growth region, and a high-density tin-nanoparticle catalyst is obtained in the growth region by electrodeposition, and the substrate is immersed in a microemulsion containing a tin salt solution, a hydrofluoric acid solution, and a surfactant during deposition. Particles having a radius of 10-20 nm.
  • the silane (PS) is thermally decomposed at 450-470 ° C to obtain silane gas; then the silane gas is used as a lead gas to grow silicon nanowires on the surface of the tin nanoparticle catalyst layer, so that the suspended electrodes are connected through the nanowire array, and the nano
  • the surface is subjected to surface modification treatment of Ba, Hf, and Zr doping to increase the surface state density and increase the surface effect and piezoresistive characteristics, as shown in FIG.
  • the oxide film on the nanowire is treated with hydrofluoric acid, the surface of the nanowire of silicon is passivated by hydrogen, and the silicon nanoparticle whose surface is passivated by hydrogen is put into a silver nitrate solution, and silver is prepared on the silicon nanowire.
  • the first step is to spin-coat the SOI wafer on the negative photoresist, and then soft-bake after coating the glue; the second step is to scan the surface of the photoresist to obtain the required nano-line pattern and device of various sizes.
  • the third step is to develop the exposed pattern, and then remove the exposed portion to complete the device structure by the DRIE technique on the top silicon; finally, remove the unexposed portion of the photoresist.
  • a lower electrode is formed on the measurement structure substrate by a photolithography, etching, and lift-off process.
  • the initial resistance of the nanowire is obtained.
  • the horizontal direction is provided by two electrodes nanowires constant current source I, two vertical electrodes provide a voltage V 0 nanowires, the nanowires to give the initial resistance D1
  • V 0 nanowires The distance between the nanowires between the two electrodes in the vertical direction, and the distance between the nanowires between the two electrodes in the horizontal direction of d0; as previously emphasized, a bias voltage is applied between the suspension electrode of the nanowire and the substrate, and the depletion is performed.
  • the pinch-off of the nanowire conductive channel forming portion can facilitate the full realization of the nanowire giant piezoresistive property.
  • the electrothermal actuator acts as a driving device to push the displacement capacitance sensor to move to the left through the insulation module, and simultaneously pulls the nanowire to the left through the insulation module, and the nanowire moves the load sensor to the left through the insulation module.
  • k s d s k f d f
  • F a k a d a + k s d s
  • k s , k a , k f are the stiffness of the nanowire, load cell, and electrothermal actuator
  • d s , d a , d f are the displacement of the nanowire, load cell, and electrothermal actuator, respectively
  • the force F generated by the electrothermal actuator a 2NEA ⁇ Tsin ⁇ , where ⁇ is the thermal expansion coefficient of silicon, ⁇ T is the average temperature of the V-shaped beam, N being the number of V-shaped beam, a is the cross sectional area of the V-beam.
  • the stiffness k s of the nanowire can be obtained by the ratio of load sensor load to displacement corresponding to the output voltage.
  • the nanowire stiffness k s F/d s
  • the nanowire stress ⁇ F/S
  • F is the load sensor load
  • S is the cross-sectional area of the nanowire.
  • the mechanical properties and electrical properties of the nanowires were measured, and the giant piezoresistive effect of the nanowires was characterized.
  • the temperature and resistivity of the sample to be tested have a direct relationship, which affects the measurement of the piezoresistive coefficient. Therefore, the temperature of the sample to be tested must be grasped before the measurement. If the temperature of the sample is not suitable for the measurement. , will affect the final piezoresistive coefficient, it must be modified based on the improved genetic algorithm wavelet neural network model, the specific process shown in Figure 11:
  • Step 1 Population initialization: randomly initialize the population, encode the link weight between the input layer and the hidden layer of the wavelet neural network, the link weight of the hidden layer to the output layer, the scaled silver and the translation factor, and generate an initial population of a certain scale. .
  • Step 2 According to the link weight, expansion and translation factor of the wavelet neural network obtained by the individual.
  • the measured piezoresistive coefficient and temperature data are input as training data, and the error between the predicted output and the target value of the system is obtained as the fitness value F after training the wavelet neural network.
  • Step 3 Perform selection, crossover and mutation operations.
  • Step 4 Determine whether the evolution is over.
  • the fitness value satisfies the relationship
  • the genetic algorithm reaches the set number of iterations. After satisfying these two conditions, the weight, scaling and translation factors of the search can be used. Wavelet neural network calculation.
  • the invention realizes the measurement of mechanical characteristics and electrical characteristics of various measurement samples through the nanowire giant piezoresistive characteristic measuring device and the MEMS measuring method thereof, and characterizes the piezoresistive coefficient. It can be extended to other types of nanowires, such as the measurement of mechanical, electrical and piezoresistive properties of metal-silicon heterojunction nanowires.

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Abstract

L'invention concerne un dispositif de mesure de propriété piézorésistive géante de nanofil et son procédé de fabrication. Le dispositif de mesure comprend : un nanofil (6) ; un capteur de température à résistance en platine (1) ; un actionneur électrothermique (2) ; un capteur de déplacement à base de mesure capacitive (3) ; une électrode (4) ; et un capteur de charge à base de mesure capacitive (9). Le capteur de température à résistance en platine (1), l'actionneur électrothermique (2), le capteur de déplacement (3) et le capteur de charge (9) sont connectés en séquence. Quatre électrodes (4) sont présentes. Les quatre électrodes (4) sont disposées entre le capteur de déplacement (3) et le capteur de charge (9). Le nanofil (6) est disposé entre deux électrodes placées horizontalement (4). Les électrodes (4) sont disposées sur un côté supérieur et un côté inférieur du nanofil (6). Le dispositif de mesure et son procédé de fabrication peuvent réaliser une mesure simultanée d'une propriété mécanique et d'une propriété électrique du nanofil (6), ce qui permet d'achever la caractérisation d'un coefficient piézorésistif. L'invention est applicable à une variété d'échantillons de mesure.
PCT/CN2016/102073 2015-11-09 2016-10-14 Dispositif de mesure de propriété piézorésistive géante de nanofil et son procédé de fabrication WO2017080340A1 (fr)

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CN104090165A (zh) * 2014-05-21 2014-10-08 南京信息工程大学 硅纳米传感阵列巨压阻系数测量系统及四点弯曲施力装置
CN105223421A (zh) * 2015-11-09 2016-01-06 南京信息工程大学 纳米线巨压阻特性测量装置及其制造方法
CN205193157U (zh) * 2015-11-09 2016-04-27 南京信息工程大学 纳米线巨压阻特性测量装置

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