CN108190829A - Preparation method based on ion implanting graphene resonant mode MEMS pressure sensor - Google Patents

Preparation method based on ion implanting graphene resonant mode MEMS pressure sensor Download PDF

Info

Publication number
CN108190829A
CN108190829A CN201711498024.4A CN201711498024A CN108190829A CN 108190829 A CN108190829 A CN 108190829A CN 201711498024 A CN201711498024 A CN 201711498024A CN 108190829 A CN108190829 A CN 108190829A
Authority
CN
China
Prior art keywords
pressure
graphene
sensitive film
sub
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711498024.4A
Other languages
Chinese (zh)
Other versions
CN108190829B (en
Inventor
张明亮
季安
王晓东
杨富华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Semiconductors of CAS
Original Assignee
Institute of Semiconductors of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Semiconductors of CAS filed Critical Institute of Semiconductors of CAS
Priority to CN201711498024.4A priority Critical patent/CN108190829B/en
Publication of CN108190829A publication Critical patent/CN108190829A/en
Application granted granted Critical
Publication of CN108190829B publication Critical patent/CN108190829B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B7/00Microstructural systems; Auxiliary parts of microstructural devices or systems
    • B81B7/02Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00349Creating layers of material on a substrate
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/10Measuring force or stress, in general by measuring variations of frequency of stressed vibrating elements, e.g. of stressed strings
    • G01L1/103Measuring force or stress, in general by measuring variations of frequency of stressed vibrating elements, e.g. of stressed strings optical excitation or measuring of vibrations
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L9/00Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
    • G01L9/0001Transmitting or indicating the displacement of elastically deformable gauges by electric, electro-mechanical, magnetic or electro-magnetic means
    • G01L9/0008Transmitting or indicating the displacement of elastically deformable gauges by electric, electro-mechanical, magnetic or electro-magnetic means using vibrations
    • G01L9/0016Transmitting or indicating the displacement of elastically deformable gauges by electric, electro-mechanical, magnetic or electro-magnetic means using vibrations of a diaphragm
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00Specific applications of microelectromechanical systems
    • B81B2201/02Sensors
    • B81B2201/0264Pressure sensors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00Manufacture or treatment of microstructural devices or systems
    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Manufacturing & Machinery (AREA)
  • Micromachines (AREA)
  • Measuring Fluid Pressure (AREA)

Abstract

Present disclose provides a kind of preparation methods based on ion implanting graphene resonant mode MEMS pressure sensor, form dielectric layer on a monocrystaline silicon substrate, and form pressure-sensitive film;Metal catalyst layer is deposited in pressure-sensitive film front, in resonance subregion Implantation of C Ion, and promotes graphene growth;Deposit etches metal to form electrical interconnection;Etch media layer, release form graphene harmonic oscillator;Glass-encapsulated cover board is made, glass-encapsulated cover board is bonded with where graphene harmonic oscillator in face of standard;Protector plate for glass is made, protector plate for glass with where the back side depth chamber of pressure-sensitive film in face of standard is bonded, is diced into separating pressure sensor chip.

Description

Preparation method based on ion implanting graphene resonant mode MEMS pressure sensor
Technical field
This disclosure relates to graphene prepares and application device processing, the processing of micro-nano electronics, MEMS making and pressure measurement neck Domain more particularly to a kind of preparation method based on ion implanting graphene resonant mode MEMS pressure sensor.
Background technology
A large amount of basic research show that graphene has excellent light, electricity, mechanical performance, for example, single-layer graphene is visible Optical band has more than 97% light transmittance, and electric conductivity and flexibility are superior to ito thin film;Electron mobility is about silicon at room temperature 140 times, and temperature stability is high;100 times of Young's modulus about 1.1TPa, about tensile strength 125GPa, steel;Thermal conductivity at room temperature About 5000Wm-1.K-1, it is 40 times of silicon, is copper more than 10 times;Etc..All these excellent properties depend on graphite The problem of alkene material preparation, large area controllable preparation high-quality graphene is always most critical in graphene research and application.With CVD method and chemical solution method are compared, and ion implantation prepares graphene using less.But ion implantation can be controlled more accurately Amount of carbon atom and position also provide more growthing process parameters for adjusting graphene quality.
It is the Golovchenko seminar of breathing out not College Physics system that earliest report prepares graphene with ion implantation, 500nm metal nickel films are deposited on silicon chip with thermooxidative layer, under the argon gas protection for being mixed with hydrogen, 1000 degrees Celsius of annealing 2 Hour.Test shows the average grain size of nickel up to 2 microns, and the main crystal face in surface is (111) face.With Varian ion implantings Machine, using 30kev Implantation Energies, dosage is respectively 2E15,4E15,7.9E15, and 1.3E16ions/cm2It (is correspondingly formed The amount of carbon atom required for 0.5,1,2, and 3 layer graphene) carry out carbon ion implantation.The sample injected is true in 5E-8Torr It is aerial to be heated to 1000 degrees Celsius, and kept for 1 hour, then, cooled down, be prepared with 5-20 centigrade per minutes cooling rate Individual layer, bilayer, three layers and a small amount of multi-layer graphene sample.Laurent Baraton of France et al. are adopted on similar substrates With 80kev Implantation Energies (corresponding carbon atom cast in nickel is 100nm), it is not 1.6E16ions/cm that dosage, which is,2Carry out carbon Ion implanting, annealed and nickel corrosion, has obtained discontinuous 4 layer graphene film.One seminar of South Korea is in similar Ni/ 20kev energy injections 1E15ions/cm is used on SiO2/Si substrates2Carbon ion, it is Celsius to be maintained at 500 for underlayer temperature during injection Degree.The sample of injection completes graphene growth under different protective atmospheres, annealing temperature, retention time, cooling rate.They send out It is existing, in the case where there is silicon dioxide layer of protection covering, good quality single-layer graphene is obtained in nickel metal layer upper surface, meanwhile, in gold Belonging to nickel lower surface also has graphene to be formed.According to another report, (2,4,5,8,10) E15ions/ is injected with 70kev energy at room temperature cm2Carbon ion enter copper sheet, vacuum annealing at 1100 degrees celsius, keep 15 minutes after, be down to 10 centigrade per minutes Room temperature, in the whole text, surface has obtained individual layer to three layer graphenes.
The country also has multiple research groups report to prepare graphene using ion implantation, representative to have Wuhan University Pay moral monarch et al. and Chinese Academy of Sciences's Shanghai micro-system Di Zengfeng et al..The seminar of Wuhan University is using carbanion or with negative The Spectra of Carbon Clusters of charge carries out ion implanting for carbon source, is growth catalyst using nickel or copper, all obtains graphene film.It is micro- System seminar using dissolubility difference of the carbon atom in nickel and copper, be catalyzed using the monel of different components Agent has obtained individual layer bilayer graphene.The work is pointed out, by controlling implantation dosage, energy, catalyst component, annealing temperature And speed, it can controllably prepare individual layer, bilayer or multilayer graphene.
Resonant mode MEMS pressure sensor is very suitable for requiring stringent aerospace, gas to high-precision and long-time stability As monitoring, industrial stokehold and other accurate measurement occasions, being widely used for it have national security, national economic development etc. Important supporting role.Resonant tube type compression transducer is high to material and manufacture craft requirement, and volume is big, signal synthesis Degree is low, to operating environment requirements, harsh, reliability and maintainability are all bad.In recent years, high-precision resonant mode MEMS pressure passes Sensor is quickly grown, and especially in high-speed flight field, there is irreplaceable status.For example, aircraft is breaking through velocity of sound process In, due to the influence of shock wave, resonant tube type compression transducer up to 700 meters, misses the measurement of angle the error of elevation carrection Difference is also up to 3 degree.For supersonic flight, so big Navigation system error may be fatal.Miniature resonance type MEMS pressure Sensor, eliminates all pressure measurement pipelines, eliminates lag error, volume and weight less than cylinder shell resonant sensor ten/ One, precision reaches full scale 4/10000ths or so, and is remained under the combined influences such as vibration, acceleration, impact, temperature and density Ensure the main precision of atmosphere data, Stealth Fighter is superior.It is reported that it is given birth to using Schlumberger airborne sensors branch company The resonant silicon microstructure pressure sensor of production makes digital air data computer, is used successfully in U.S.'s F22 opportunities of combat, adopts With advanced distributed measurement array, there is especially excellent pneumatic and stealthy advantage, the flight product of opportunity of combat have been effectively ensured Matter and operational performance.
Resonant mode MEMS pressure sensor causes harmonic oscillator resonant frequency to change based on pressure, pressure is measured indirectly, with biography System pressure sensor is compared, it has many advantages, such as, and small, low in energy consumption, precision is high, stability is good and exports quasi- digital signal.It is humorous Oscillator is the core of resonant mode MEMS pressure sensor, its material, configuration, size, excitation detection mode etc. directly determine Device performance.At present, monocrystalline silicon is still the optimal material for making harmonic oscillator.
Silicon substrate resonant mode MEMS pressure sensings are developed by the Druck companies of Britain of GE corporate buyouts of the U.S. earliest Device, RTP series and DPS8000 series of products are currently the highest pressure sensor of nominal accuracy in the world.Due to manufacture craft Complexity, product cost is higher, at present, each about 2000 dollars of external price of sensor.Japanese Yokogawa Motor strain formula can be developed The resonant mode high-precision pressure sensor of a electromagnetic excitation electromagnetic detection, monocrystalline silicon harmonic oscillator Q values reach 50000, full scale Precision is up to 0.01%, 10ppm/ DEG C of temperature coefficient, year stability be 100ppm full scales.French Thales companies, Schlumberger airborne sensors branch company, Honeywell Corp. USA, Industrial Research Limited of New Zealand, Sweden look into Er Musi Polytechnics, Sweden's Royal Institute of Technology etc. all reported that silicon resonance type Study on pressure sensor worked, in the market Their product was not met.
Domestic Northwestern Polytechnical University's sky day micro-nano system laboratory is in silicon substrate resonance type pressure sensor optimization design, system Make, report many achievements in terms of performance test.Sensing technology National Key Laboratory of electronics research institute of the Chinese Academy of Sciences also develops Go out a series of high-precision resonant mode MEMS pressure sensors.BJ University of Aeronautics & Astronautics's instrumental science and the micro- biography of photoelectric project institute Feel technology experiment room, Xiamen University's physics and Electrical and Mechanical Engineering College, College of Information Science and Engineering of Shenyang University of Technology, China's electricity The 49th research institute of scarabaeidae skill group company, National University of Defense Technology's electromechanical engineering and Automation Institute etc., all reported that silicon was humorous Formula of shaking Study on pressure sensor.
Up to the present, it is not yet reported that both at home and abroad, injects ions into the graphene being prepared in situ and be fabricated to resonant mode MEMS pressure sensor.
Invention content
(1) technical problems to be solved
To solve technical problem of the existing technology, present disclose provides one kind to be based on ion implanting graphene resonant mode The preparation method of MEMS pressure sensor.
(2) technical solution
Present disclose provides a kind of preparation method based on ion implanting graphene resonant mode MEMS pressure sensor, packets It includes:Step S101:Dielectric layer is formed on a monocrystaline silicon substrate, and forms pressure-sensitive film;Step S201:It forms sediment in pressure-sensitive film front Product metal catalyst layer, in resonance subregion Implantation of C Ion, and promotes graphene growth;Step S301:Deposit etching metal To form electrical interconnection;Etch media layer, release form graphene harmonic oscillator;Step S401:Glass-encapsulated cover board is made, by glass Glass encapsulation cover plate is bonded with where graphene harmonic oscillator in face of standard;Step S501:Make protector plate for glass, by protector plate for glass with In face of quasi- bonding where the back side depth chamber of pressure-sensitive film, it is diced into separating pressure sensor chip.
In some embodiments of the present disclosure, the step S101 includes:Sub-step S101a:It gives birth on a monocrystaline silicon substrate Long dielectric layer material forms dielectric layer;Sub-step S101b:Define size and the position of pressure-sensitive film, etch media layer, shape Into the mask layer for making pressure-sensitive film;Sub-step S101c:Form pressure-sensitive film.
In some embodiments of the present disclosure, the step S201 includes:Sub-step S201a:It forms sediment in pressure-sensitive film front Product metal catalyst layer, for growing graphene;Sub-step S201b:Using photoresist as mask, in resonance subregion ion implanting Carbon;Sub-step S201c:High annealing promotes graphene growth into patterned graphene.
In some embodiments of the present disclosure, the step S301 includes:Sub-step S301a:Deposit thickeies metal layer, carves Metal layer is lost, forms electrical interconnection;Sub-step S301b:Etch media layer, release form graphene harmonic oscillator.
In some embodiments of the present disclosure, in the sub-step S101a, using low-pressure chemical vapor deposition, high temperature Oxidation, ion beam sputtering, plasma enhanced chemical vapor deposition technique one of which somatomedin layer material.
In some embodiments of the present disclosure, dielectric layer material is silicon nitride, silica or combination thereof, and thickness is 100nm-5μm。
In some embodiments of the present disclosure, in the step S101b, pressure-sensitive film is defined using photoetching process Size and position, then using photoresist as mask, using dry or wet etch dielectric layer, form the mask of pressure-sensitive film Layer.
In some embodiments of the present disclosure, in the step S101c, pass through dry etching or wet etching or combination Technique, etches back side depth chamber, and remaining monocrystalline silicon thin film is pressure-sensitive film.
In some embodiments of the present disclosure, in the sub-step S201a, using electron beam evaporation, magnetron sputtering, electricity The one of which deposit metal catalyst layer of plating;In the sub-step S201c, promoted in a vacuum or in protective gas Make the high-temperature annealing process of graphene growth.
In some embodiments of the present disclosure, in the sub-step S301a, electrical interconnection is defined using photoetching process Figure using wet processing, dry process or combination thereof etching sheet metal, forms the electrical interconnection of definition.
(3) advantageous effect
It can be seen from the above technical proposal that the disclosure has the advantages that:
1st, the disclosure is since preparation method is using photoetching process, etching technics and thin-film technique, can effectively with CMOS works Skill is compatible with, and can be produced in batches.
2nd, graphene can be made in situ with ion implanting, using the disclosure with reference to glass cover-plate and protector plate for glass, system Graphene resonant mode MEMS pressure sensor is made, for accurately measuring pressure.
Description of the drawings
Fig. 1 shows somatomedin layer on a monocrystaline silicon substrate.
Fig. 2 shows the mask layer for forming pressure-sensitive film.
Fig. 3, which is shown, produces pressure-sensitive film.
Fig. 4 shows deposit metal catalyst layer.
Fig. 5 is shown carries out carbon ion implantation by mask of photoresist.
Fig. 6 shows the graphene for growing and defining figure.
Fig. 7 shows thickening metal layer and forms electrical interconnection.
Fig. 8 shows that etch media layer discharges graphene harmonic oscillator.
Fig. 9 shows that glass-encapsulated cover board is bonded with harmonic oscillator.
Figure 10 shows that glass-encapsulated cover board is bonded with pressure-sensitive film back side depth Cavity surface.
Figure 11 is preparation method stream of the embodiment of the present disclosure based on ion implanting graphene resonant mode MEMS pressure sensor Cheng Tu.
Specific embodiment
For graphene micro-nano device it has been reported that very much, most device performances are not up to theory expectation, are largely determined by stone The influence of black alkene quality of materials and device manufacturing process.The disclosure uses ion implantation, controllable preparation large-area high-quality Graphene by micro-nano technology technique in situ, produces graphene resonant mode MEMS pressure sensor.High-precision resonant mode MEMS pressure sensor application demand is very big, the resonant mode MEMS pressure sensor reported both at home and abroad, is all using monocrystalline silicon Harmonic oscillator is made, the good commercial devices of only several precision high stabilities buy difficulty, and somewhat expensive in China.This public affairs It opens the graphene resonant mode MEMS pressure sensor country being related to and was showed no similar report.
Purpose, technical scheme and advantage to make the disclosure are more clearly understood, below in conjunction with specific embodiment, and reference The disclosure is further described in attached drawing.It should be noted that in attached drawing or specification description, similar or identical portion Divide and all use identical figure number.The realization method for not being painted or describing in attached drawing is those of ordinary skill in technical field Known mode.In addition, though the demonstration of the parameter comprising particular value can be provided herein, it is to be understood that parameter is without definite Equal to corresponding value, but can be similar to be worth accordingly in acceptable error margin or design constraint.
Please also refer to Fig. 1 to Figure 10, the embodiment of the present disclosure provides a kind of based on ion implanting graphene resonant mode The preparation method of MEMS pressure sensor, referring to Figure 11, this method includes:
Step S101:Dielectric layer is formed on a monocrystaline silicon substrate, and forms pressure-sensitive film.
The step specifically includes:
Sub-step S101a:The somatomedin layer material in monocrystalline substrate 100 forms dielectric layer 101, feels for making The mask layer of ironed film, as shown in Figure 1.Monocrystalline substrate 100 can be arbitrary thickness, arbitrary high preferred orientation, arbitrary Resistivity;Dielectric layer material can be silicon nitride, silica or combination thereof, and low pressure may be used in 100nm-5 μm of thickness It is prepared by the similar techniques such as chemical vapor deposition, high-temperature oxydation, ion beam sputtering, plasma enhanced chemical vapor deposition.
Sub-step S101b:Size and the position of pressure-sensitive film are defined, etch media layer 101 forms pressure-sensitive film Mask layer 102, as shown in Figure 2.Define size and the position of pressure-sensitive film using photoetching process, then using photoresist to cover Film using dry or wet etch dielectric layer 101, forms the mask layer of pressure-sensitive film.
Sub-step S101c:Pressure-sensitive film 103 is formed, as shown in Figure 3.Pass through dry etching or wet etching or combination work Skill, etches back side depth chamber 104, and remaining monocrystalline silicon thin film is pressure-sensitive film.After experiencing pressure shape occurs for pressure-sensitive film Become, by the clamped anchor point on pressure-sensitive film, the resonant frequency in stress transfer to harmonic oscillator, causing harmonic oscillator is changed; Resonance type pressure sensor reads the pressure experienced on pressure-sensitive film by measuring the variation of harmonic oscillator resonant frequency;Pressure-sensitive The thickness and size of film determine the range of sensor, and influence the performance indicators such as sensitivity, sluggishness, non-linear;According to week The clamped diaphragm stress model in side calculates stress and deformation quantity that pressure-sensitive film is each put;Referred to according to the technology of pressure sensor Mark requirement, determines the thickness and shape of pressure-sensitive film, sets position and size of the anchor point on pressure-sensitive film;Pressure-sensitive film can To be flat diaphragm or carry the folding diaphragm of stress concentration structure.
Step S201:Metal catalyst layer is deposited in pressure-sensitive film front, in resonance subregion Implantation of C Ion, and is promoted Graphene growth.
The step specifically includes:
Sub-step S201a:Metal catalyst layer 105 is deposited in pressure-sensitive film front, for growing graphene, such as Fig. 4 institutes Show.Catalyst metals include the one kind such as copper, nickel, cobalt, titanium, aluminium, iron, molybdenum, tungsten, gold, platinum, palladium, ruthenium, rhodium or several or combination is closed Gold and associated metal;Depositing technics can be the technique of the similar generation metallic film such as electron beam evaporation, magnetron sputtering, plating; The thickness of metal catalyst layer is 50nm-2 μm;In order to increase the crystallinity of metal and metal surface and metal medium bed boundary Planarization generally under argon gas, nitrogen, hydrogen or their gaseous mixture protective atmosphere, carries out thermal annealing;Annealing temperature and when Between selected according to different types of metal, it is final so that metal has more even curface and the crystalline particle of bigger.
Sub-step S201b:It is mask with photoresist 106, in resonance subregion Implantation of C Ion 107, as shown in Figure 5.It is logical The mode of ion implanting is crossed, the carbon atom for being used to form graphene is quantitatively adding in metal catalyst layer.Form mono-layer graphite Alkene about needs 4E15cm-2Carbon implantation dosage, according to the graphene number of plies that desirably forms, set total carbon implantation dosage.According to carbon Cast of the atom in different metal is different, Implantation Energy is adjusted slightly, in order to carbon migration to metal catalyst layer Surface or interface form graphene;The shape and size of harmonic oscillator, in anharmonic oscillator region, carbon atom are defined with photoetching process It all rests in 106 mask of photoresist, there is no carbon atom in metal catalyst layer, graphene will not be grown.
Sub-step S201c:High annealing promotes graphene growth into patterned graphene 108, as shown in Figure 6.True High-temperature annealing process that is aerial or carrying out promoting graphene growth in protective gas, protective gas is argon gas, nitrogen or mixed The gaseous mixture of hydrogen;Annealing temperature, heating rate, cooling rate, soaking time are adjusted according to different metal catalyst system, For example, for copper, under high-purity argon gas protection, about 5 DEG C/min of general warming and cooling rate is kept the temperature in 1100 DEG C of about 30min;For Nickel under condition of similarity, is kept the temperature at 900 DEG C;For relatively thin metal catalyst layer, carbon atom can both move to metal and urge Agent layer surface, on the interface that can also move to metal catalyst layer and dielectric layer, two sides can form graphene;For thickness Metal catalyst layer, using small Implantation Energy, graphene can be formed in metallic catalyst layer surface;Using big injection energy Amount, graphene are more likely to grow on the interface of metal catalyst layer and dielectric layer.
Step S301:Deposit etches metal to form electrical interconnection;Etch media layer, release form graphene harmonic oscillator.
The step specifically includes:
Sub-step S301a:Deposit thickeies metal layer 109, and etching sheet metal 109 forms electrical interconnection 110, such as Fig. 7 institutes Show.Since graphene grows out in metal catalyst layer surface catalysis, another function of metal catalyst layer is straight It connects and forms ohm electrical contact with graphene;If the thinner thickness of metal catalyst layer, it is also necessary to thicken, the thickness of metal layer General about 1 μm just can guarantee reliable metal interconnection;The figure of electrical interconnection is defined using photoetching process, using wet processing, Dry process or combination thereof etching sheet metal form the electrical interconnection of definition.
Sub-step S301b:Etch media layer, forming layer 111, release forms graphene harmonic oscillator, as shown in figure 8, described Layer 11 is discontinuous dielectric layer.Harmonic oscillator oscillating component needs are thoroughly hanging, provide free vibration space;Determined with photoetching process Justice needs hanging region, and the dielectric layer of support graphene is etched using wet processing, dry process or combination thereof;If stone Black alkene is grown in metallic catalyst surfaces, and after metal layer is partially etched, graphene may be suspended;For certain knots The harmonic oscillator of structure, if the space of free vibration is enough, this step process can not be done.
Step S401:Glass-encapsulated cover board is made, glass-encapsulated cover board is bonded with where graphene harmonic oscillator in face of standard.
In this step, glass-encapsulated cover board 112 is made, by glass cover-plate 113 and graphene with through hole electrode 113 It is bonded where harmonic oscillator in face of accurate, as shown in Figure 9.Graphene harmonic oscillator needs work in a vacuum, using glass silicon anode key It closes, structure vacuum sealing vibration cavity.Another effect of glass cover-plate is to provide electrical signal access to graphene harmonic oscillator. This disclosure relates to resonance type pressure sensor in, graphene harmonic oscillator is encouraged by electrostatic force, piezoresistive detection read harmonic oscillator Resonant frequency.There are vibration cavity, through-electrode, through-hole, getter (can not for certain structures on glass-encapsulated cover board With);Vibration cavity is located at right over harmonic oscillator, provides free movement space;Through-electrode provides static electric excitation signal, Ke Yishi Metal packed column or monocrystalline silicon column;Through-hole is located above pressure drag pad, and as electrical interconnection lead, shape is usually taper; Fe Getter Films Prepared is deposited in vibration cavity, keeps vacuum degree higher in sealing vacuum chamber;The making work of glass-encapsulated cover board Skill includes:Photoetching process defines the position of figure and size, wet-dry change etch to form vibration cavity and alignment mark, laser boring Through-hole, magnetron sputtering or electron beam evaporation deposit Fe Getter Films Prepared, plating is formed to prepare metal column filling, glass reflux, combine CMP grinding and polishings make silicon column through hole electrode in glass.Glass-encapsulated cover board carries out being directed at anode key with graphene harmonic oscillator face It closes, forms vacuum sealing simultaneously, construct the electrical stimuli and read-out electrode of harmonic oscillator.
Step S501:Protector plate for glass is made, by face alignment keys where the back side depth chamber of protector plate for glass and pressure-sensitive film It closes, is diced into separating pressure sensor chip.
In this step, protector plate for glass 114 is made, it will be where the back side depth chamber of protector plate for glass 114 and pressure-sensitive film It is bonded in face of standard, is diced into separating pressure sensor chip, as shown in Figure 10.The effect of protector plate for glass has two aspects:When Pressure-sensitive film is protected not to be damaged;Second is that the internal stress of the whole chip of balance.It, will be tested with through-hole on protector plate for glass The pressure of amount is transmitted to by gas or inert fluid on pressure-sensitive film, realizes pressure measurement.Protector plate for glass uses laser Punching makes through-hole, and CMP grinding and polishings adjust the thickness of protector plate for glass so that after three layers of bonding of glass-silicon-glass in chip Portion's stress is minimum;Protector plate for glass is aligned with chip pressure-sensitive film back side depth Cavity surface by anode linkage and is combined together;Chip Double-face adhesive adhesive film is protected, the standalone feature chip detached using grinding wheel or laser scribing means scribing.
The disclosure is further described below by way of an example.
1. by the use of double n-Si (100) monocrystalline silicon of throwing of 360 microns of thickness as substrate, first thermal oxide is thick in two-sided 1 micron of growth Silica, then with low-pressure chemical vapor deposition in two-sided growth richness nitrogen silicon nitride 300nm.
2. carry out photoetching process with AZ6130 photoresists, then using photoresist as mask, using dry method exposure silicon nitride and Silica until monocrystalline silicon surface, forms the mask layer of pressure-sensitive film.
3. after cleaning up photoresist, the Protection glue BK-2 of anti-KOH corrosion is applied in the one side for not making photoetching, is put into 80 DEG C In 30% KOH aqueous solutions, corrosion forms 330 microns of deep chamber, leaves 30 microns thick of monocrystalline silicon pressure-sensitive film.
4. after RCA is cleaned, silicon nitride is removed in concentrated phosphoric acid, then clean, be put into electron beam evaporation, it is thin in pressure-sensitive Film front deposits 300nm metallic nickels.Using the nitrogen for being mixed with hydrogen as protection gas, anneal 30 minutes at 1000 DEG C, promote metallic nickel The crystal grain and more even curface of formation bigger and metal silicon/silicon dioxide interface.
5. carrying out photoetching process with AZ6130 photoresists, exposing needs the region to form graphene, in Varian 300XP With 30kev energy injection carbon ions 1E16cm on ion implantation apparatus-2Accumulated dose.
6. cleaning removal photoresist, under the nitrogen protection for being mixed with hydrogen, warming and cooling rate is 5 DEG C/min, in 900 DEG C of guarantors Warm 30min forms the graphene for defining pattern in metal nickel surface.
7. deposited by electron beam evaporation deposits 50nm metallic nickels, good Ohmic contact is formed with graphene, then deposits thickening gold Belong to 1 micron of aluminium.Photoetching, wet etching metallic aluminium and metallic nickel form the electrical interconnection of definition.
8. using thick resist lithography, the silica for needing to erode is exposed, using dry etching plus wet etching, removal Silica below graphene harmonic oscillator provides sufficient room for harmonic oscillator free vibration.
9. preparing glass through-hole silicon electrode using glass technique of backflow, then produce the sky that harmonic oscillator free vibration is provided Chamber deposits Fe Getter Films Prepared in cavity, and glass cover-plate carries out alignment anode linkage with graphene harmonic oscillator face, and it is close to form vacuum Envelope simultaneously, constructs the electrical stimuli and reading circuit of harmonic oscillator.
10. 300 microns of thick sheet glass is selected to do protector plate for glass, position making through-hole is being defined with laser boring, is being led to It crosses anode linkage and is aligned with chip pressure-sensitive film depth Cavity surface and is combined together.Chip double-side patch adhesive film protection, is drawn using grinding wheel The standalone feature chip that piece machine scribing is detached.
Particular embodiments described above has carried out the purpose, technical solution and advantageous effect of the disclosure further in detail It describes in detail bright, it should be understood that the foregoing is merely the specific embodiment of the disclosure, is not limited to the disclosure, it is all Within the spirit and principle of the disclosure, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the disclosure Within the scope of shield.

Claims (10)

1. based on the preparation method of ion implanting graphene resonant mode MEMS pressure sensor, including:
Step S101:Dielectric layer is formed on a monocrystaline silicon substrate, and forms pressure-sensitive film;
Step S201:Metal catalyst layer is deposited in pressure-sensitive film front, in resonance subregion Implantation of C Ion, and promotes graphite Alkene is grown;
Step S301:Deposit etches metal to form electrical interconnection;Etch media layer, release form graphene harmonic oscillator;
Step S401:Glass-encapsulated cover board is made, glass-encapsulated cover board is bonded with where graphene harmonic oscillator in face of standard;
Step S501:Protector plate for glass is made, protector plate for glass with where the back side depth chamber of pressure-sensitive film in face of standard is bonded, is drawn Piece ingredient tripping sensor chip.
2. preparation method as described in claim 1, the step S101 includes:
Sub-step S101a:Somatomedin layer material on a monocrystaline silicon substrate forms dielectric layer;
Sub-step S101b:Define size and the position of pressure-sensitive film, etch media layer forms the mask of pressure-sensitive film Layer;
Sub-step S101c:Form pressure-sensitive film.
3. preparation method as described in claim 1, the step S201 includes:
Sub-step S201a:Metal catalyst layer is deposited in pressure-sensitive film front, for growing graphene;
Sub-step S201b:Using photoresist as mask, in resonance subregion Implantation of C Ion;
Sub-step S201c:High annealing promotes graphene growth into patterned graphene.
4. preparation method as described in claim 1, the step S301 includes:
Sub-step S301a:Deposit thickeies metal layer, and etching sheet metal forms electrical interconnection;
Sub-step S301b:Etch media layer, release form graphene harmonic oscillator.
5. preparation method as claimed in claim 2, in the sub-step S101a, using low-pressure chemical vapor deposition, high temperature Oxidation, ion beam sputtering, plasma enhanced chemical vapor deposition technique one of which somatomedin layer material.
6. preparation method as claimed in claim 5, dielectric layer material is silicon nitride, silica or combination thereof, thickness It is 100nm-5 μm.
7. in the step S101b, pressure-sensitive film is defined using photoetching process for preparation method as claimed in claim 2 Size and position, then using photoresist as mask, using dry or wet etch dielectric layer, form the mask of pressure-sensitive film Layer.
8. preparation method as claimed in claim 2 in the step S101c, passes through dry etching or wet etching or group Technique is closed, etches back side depth chamber, remaining monocrystalline silicon thin film is pressure-sensitive film.
9. preparation method as claimed in claim 3, in the sub-step S201a, using electron beam evaporation, magnetron sputtering, The one of which deposit metal catalyst layer of plating;
In the sub-step S201c, in a vacuum or in protective gas promote the high annealing work of graphene growth Skill.
10. in the sub-step S301a, electrical interconnection is defined using photoetching process for preparation method as claimed in claim 4 Figure, using wet processing, dry process or combination thereof etching sheet metal, form the electrical interconnection of definition.
CN201711498024.4A 2017-12-29 2017-12-29 Preparation method of resonant MEMS pressure sensor based on ion implantation graphene Active CN108190829B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711498024.4A CN108190829B (en) 2017-12-29 2017-12-29 Preparation method of resonant MEMS pressure sensor based on ion implantation graphene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711498024.4A CN108190829B (en) 2017-12-29 2017-12-29 Preparation method of resonant MEMS pressure sensor based on ion implantation graphene

Publications (2)

Publication Number Publication Date
CN108190829A true CN108190829A (en) 2018-06-22
CN108190829B CN108190829B (en) 2020-12-15

Family

ID=62587649

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711498024.4A Active CN108190829B (en) 2017-12-29 2017-12-29 Preparation method of resonant MEMS pressure sensor based on ion implantation graphene

Country Status (1)

Country Link
CN (1) CN108190829B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110031133A (en) * 2018-11-12 2019-07-19 罕王微电子(辽宁)有限公司 A kind of resonance type pressure sensor and manufacture craft
CN110686809A (en) * 2019-10-10 2020-01-14 南京大学 Pressure sensor based on double-layer graphene and preparation method
CN111579147A (en) * 2020-05-29 2020-08-25 中国科学院半导体研究所 Resonant MEMS differential pressure sensor and preparation method thereof
CN113044806A (en) * 2021-03-12 2021-06-29 大连理工大学 MEMS device monolithic integration structure for realizing pressure sensing and method thereof
CN116676584A (en) * 2023-06-01 2023-09-01 北京理工大学 Preparation method of high-Q-value micro-shell harmonic oscillator graphene film

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101614604A (en) * 2009-07-14 2009-12-30 西北工业大学 Based on silicon resonance type pressure transducer of synovial membrane difference structure and preparation method thereof
CN102243990A (en) * 2011-06-21 2011-11-16 中国科学院上海微系统与信息技术研究所 Preparation method of graphite nanoribbon
CN102315831A (en) * 2011-05-04 2012-01-11 西安电子科技大学 Preparation method for nano-electromechanical resonator based on graphene
CN103296991A (en) * 2013-04-28 2013-09-11 电子科技大学 Graphene high-frequency nanomechanical resonator based on flexible substrate and preparing technology of graphene high-frequency nanomechanical resonator
US20130256627A1 (en) * 2009-06-24 2013-10-03 Lehigh University Sensors Incorporating Freestanding Carbon NanoStructures
CN104038173A (en) * 2014-06-10 2014-09-10 电子科技大学 Method for preparing graphene high frequency nano electro mechanical system (NEMS) on the basis of flexible substrate
CN106017751A (en) * 2016-05-25 2016-10-12 东南大学 High-sensitivity piezoresistive pressure sensor and preparation method thereof
CN106918420A (en) * 2017-04-21 2017-07-04 北京航空航天大学 A kind of pair of Graphene resonance beam type pressure sensor
CN107318076A (en) * 2017-06-26 2017-11-03 上海集成电路研发中心有限公司 A kind of MEMS acoustic sensors based on graphene and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130256627A1 (en) * 2009-06-24 2013-10-03 Lehigh University Sensors Incorporating Freestanding Carbon NanoStructures
CN101614604A (en) * 2009-07-14 2009-12-30 西北工业大学 Based on silicon resonance type pressure transducer of synovial membrane difference structure and preparation method thereof
CN102315831A (en) * 2011-05-04 2012-01-11 西安电子科技大学 Preparation method for nano-electromechanical resonator based on graphene
CN102243990A (en) * 2011-06-21 2011-11-16 中国科学院上海微系统与信息技术研究所 Preparation method of graphite nanoribbon
CN103296991A (en) * 2013-04-28 2013-09-11 电子科技大学 Graphene high-frequency nanomechanical resonator based on flexible substrate and preparing technology of graphene high-frequency nanomechanical resonator
CN104038173A (en) * 2014-06-10 2014-09-10 电子科技大学 Method for preparing graphene high frequency nano electro mechanical system (NEMS) on the basis of flexible substrate
CN106017751A (en) * 2016-05-25 2016-10-12 东南大学 High-sensitivity piezoresistive pressure sensor and preparation method thereof
CN106918420A (en) * 2017-04-21 2017-07-04 北京航空航天大学 A kind of pair of Graphene resonance beam type pressure sensor
CN107318076A (en) * 2017-06-26 2017-11-03 上海集成电路研发中心有限公司 A kind of MEMS acoustic sensors based on graphene and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SHENGWEI JIANG ET AL.: ""Potential application of graphene nanomechanical resonator as pressure sensor"", 《SOLID STATE COMMUNICATIONS》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110031133A (en) * 2018-11-12 2019-07-19 罕王微电子(辽宁)有限公司 A kind of resonance type pressure sensor and manufacture craft
CN110686809A (en) * 2019-10-10 2020-01-14 南京大学 Pressure sensor based on double-layer graphene and preparation method
CN111579147A (en) * 2020-05-29 2020-08-25 中国科学院半导体研究所 Resonant MEMS differential pressure sensor and preparation method thereof
CN113044806A (en) * 2021-03-12 2021-06-29 大连理工大学 MEMS device monolithic integration structure for realizing pressure sensing and method thereof
CN113044806B (en) * 2021-03-12 2024-01-05 大连理工大学 MEMS device monolithic integrated structure for realizing pressure sensing and method thereof
CN116676584A (en) * 2023-06-01 2023-09-01 北京理工大学 Preparation method of high-Q-value micro-shell harmonic oscillator graphene film

Also Published As

Publication number Publication date
CN108190829B (en) 2020-12-15

Similar Documents

Publication Publication Date Title
CN108190829A (en) Preparation method based on ion implanting graphene resonant mode MEMS pressure sensor
CN104122014B (en) Power detecting element and power conversion element
Fang et al. Gas sensing properties of NiO/SnO2 heterojunction thin film
CN103712720B (en) Capacitance pressure transducer, and inertial sensor integrated device and forming method thereof
Bernstein et al. High Q diamond hemispherical resonators: Fabrication and energy loss mechanisms
Luo et al. Nanocrystalline SnO2 film prepared by the aqueous sol–gel method and its application as sensing films of the resistance and SAW H2S sensor
CN106441650B (en) A kind of diaphragm pressure sensor and preparation method
CN101922984A (en) Nano-silicon thin-membrane four-island-beam-membrane sensor chip and preparation method thereof
CN104297520A (en) Monolithic embedded integrated silicon acceleration and pressure composite sensor
CN106197718A (en) A kind of film temperature sensor and preparation method
CN107328449B (en) A kind of thermoelectric pile formula gas flow sensor and preparation method thereof
CN105547464B (en) MEMS piezoelectric vector hydrophone with cascaded structure and preparation method thereof
CN104142359B (en) A kind of MEMS gas sensor and processing method thereof
CN105181231A (en) Pressure sensor of packaging structure and preparation method thereof
CN103644999A (en) Low-range and high-sensitivity micro-electromechanical system (MEMS) pressure sensor and manufacture method thereof
CN109764998A (en) A kind of diaphragm type graphene MEMS micro-pressure sensor chip and preparation method thereof
CN108931321A (en) Beam-island-film integration resonant mode pressure sensor structure and manufacturing method
CN101472212B (en) Post-CMOS capacitance silicon-based micro-microphone and preparation method thereof
CN204129000U (en) A kind of MEMS gas sensor
Völklein et al. Microchip for the measurement of seebeck coefficients of single nanowires
JPH06208837A (en) Plasma drawing grid of ion beam processor
Li et al. Ultra-small high‐temperature pressure sensor chips fabricated in single‐layer (111) SOI wafers
CN207007876U (en) Quartz pendulous accelerometer
CN115683406A (en) Silicon-based film pressure-sensitive element and preparation method thereof
CN111579147B (en) Resonant MEMS differential pressure sensor and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant