CN106840476B - The quick sensing element of three-dimensional carbon nanomaterial field-effect flexible force and preparation method - Google Patents
The quick sensing element of three-dimensional carbon nanomaterial field-effect flexible force and preparation method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 118
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring 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
- G01L9/08—Measuring 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 by making use of piezoelectric devices, i.e. electric circuits therefor
Abstract
The quick sensing element of flexible force the present invention relates to one kind based on continuous three-dimensional grapheme or carbon nanotube field-effect structure designs and prepares method.The sensing element is changed using the field-effect conductance of elastomeric edges pricker bar belt surface graphene or carbon nanotube under constant grid potential is covered on, designing grid is the planar flexible electrode for being covered on graphene or carbon nanotube pyramid band or array top, grid to make under pyramid compressive deformation source drain channel area increase, and field-effect conductance increases, very high deformation or load sensitivity is presented in element.By designing strip width, array density, base elastomer body elasticity modulus of materials, load measurement range 0 can be obtained and arrive the quick sensing element of power of different sensitivity within the scope of 3MPa, and can design and be prepared into transparency higher than 80%, the quick sense film of power of the bending curvature less than 3 millimeters.
Description
Technical field
The invention belongs to electronic information fields, more particularly to the quick sensing element of a kind of carbon nanomaterial flexible force and preparation side
Method.
Background technique
The quick sensing element of flexible force is widely used in various fields, such as is used for complex-curved surface in robot field
The touch sensor of contact load perception, field of biomedicine body surface tension or antiotasis sensor and information display neck
Quick touch screen of domain power etc. obtains load with different sensing principles and senses physical quantity by being matrix using polymer material
Corresponding relationship.The quick sensing element of flexible force practical at present is substantially that polymeric piezoelectric material Kynoar (PVDF) is thin
Film, such force sensing element needs to carry out preposition amplification to signal due to weak output signal, therefore noise is smaller, to ambient noise
Inhibition there are certain requirements, and since piezoelectric effect has larger relaxation property, have larger uncertainty to the quantitative measurment of load.Closely
Nian Lai, many scholars, which have studied, prepares the quick sensing element of flexible force using various nano materials, such as is prepared using carbon nanotube
Resistance-type drawing, the quick sensing element of the quick sensing element of pressure, zinc oxide nanowire preparation piezoelectric type nanometer power, micrometer structure surface electricity
Appearance formula or the quick sensing element of field-effect tubular type power etc..
Graphene is as a kind of two-dimensional material, the electrical properties with many brilliances, high carrier mobility and low temperature
Degree sensibility makes graphene be used for a variety of fieldtrons, and since graphene has outstanding bending flexibility and visible
Optical clarity, therefore using the flexibility and field-effect characteristic of graphene, the quick sensing element of power is designed, is had than utilizing other principles
Higher sensitivity and signal-to-noise ratio, and the available higher transparency have the condition applied to a variety of flexible force sensing elements.
Using graphene as the flexible structure of field-effect sensitive material, attempted in recent years using the dielectric material conduct of organic ion colloid
Dielectric layer can make graphene field effect first since this kind of organic ion colloid dielectric material has very big dielectric constant
Part works under lower grid voltage, preferably avoids the dielectric layer as caused by high gate voltage and deformation from puncturing or leak electricity, guarantees field
Field effect transistor devices can work under multiple deformation.
Carbon nanotube scene effect on-off ratio, deformation stability, chemical stability aspect and the graphene phase of semi-conductor type
Than there is certain superiority.Field-effect force-sensing sensor is prepared using semiconductor type carbon nano-tube, there is spirit more higher than graphene
Sensitivity and deformation stability guarantee that FET device has high duplication under multiple deformation.Semi-conductor type carbon nanometer
The separation and preparation technology of pipe has physical method and chemical method, and the metal and semi-conductor type that can be prepared from batch chemical vapor deposition are mixed
It closes in object and isolates semiconductor type carbon nano-tube.
Present invention pyramid band minus structure on three-dimensional Copper substrate by design, uses chemical vapor deposition method on it
The controllable graphene single-layer or multi-layer film of thickness is prepared, then transfers graphene to elastomer eurymeric surface with transfer method, or straight
It connects and coats semiconductor type carbon nano-tube on elastomer eurymeric surface, use silver or copper nano-wire as source, drain conducting electrodes, with covering
It is dielectric layer in graphene or the Ionic colloid of carbon nano tube surface, to be covered on carbon nanotube, the silver of polymeric film surface
Nano wire or copper nano-wire are conductive grid, and grid conducting layer is contacted with pyramid tips, forms parallel removable gate field
Effect transistor structure the source-drain current of the structure and is applied to grid to pyramid when bias is fixed between grid voltage and source and drain
Compressive deformation is proportional, by designing the support construction between different pyramid band and grid and pyramid band, can design
The quick sensing element of the power of different loads sensitive range.
Since above structure pyramid size can achieve 20 microns, there is integration, single pyramid naked eyes are not easy to differentiate,
Graphene and nano line electrode have high transparency, therefore above structure is suitble to be also used to the higher flexible force of transparency requirement
Quick touch screen and other force sensing elements.In the application of less demanding to the transparency, can be obtained using wider pyramid size
It can be designed that a variety of different loads measure to more Large strain sensitivity and more high dynamic range, therefore by above-mentioned basic structure
The force sensing element of range, has a wide range of applications.
Summary of the invention
It is an object of the present invention to provide a kind of design, highly sensitive, high stability flexible force sensitive sensor method is prepared,
Sensor sensitivity within the scope of 0 to 3MPa can be designed by structural adjustment, and maximum sensitivity can achieve 3MPa-1, there is high-temperature, strain stable, minimum dimension can be wide to 20 microns, and it is thin less than 3 millimeters to can be made into transparent, bending curvature
Membrane forces sensing structure.
The technical scheme is that；Flexible force quick sensing element of the one kind based on three-dimensional carbon nanomaterial fet structure
Part is made of centrum layer and the conductive gate layer being covered on centrum layer；The centrum layer is followed successively by elasticity by center outward
Body three-dimensional rib body bores film layer, carbon nanomaterial film layer, parallel strip-like electrodes layer, Ionic colloid dielectric materials layer；The bullet
Property body three-dimensional rib body cone film layer be several three-dimensional rib body tapers at parallel one-dimensional pyramid band or array, the three-dimensional rib body
20-150 microns of the bottom width of cone；The matrix of the conductive gate layer is elastomeric material, and surface covers flexible conducting material, leads
The tip contact of the three-dimensional rib body cone of material layer and centrum layer, forms removable field effect transistor gate；The carbon is received
Rice material film layers are continuous graphite alkene or dispersing Nano carbon tubes.
The elastomer three-dimensional rib body cone film layer material is room curing silicon rubber, thermoplastic polyurethane, Etheric ester type heat
Any one in thermoplastic elastic.
The Ionic colloid dielectric materials layer be the double fluoroform semi-annular jade pendant imide salts ionic liquids of 1- ethyl-3-methylimidazole with
The mixture of vinylidene fluoride-hexafluoropropylene copolymer is deposited on carbon nanomaterial thin-film surface with solution lacquering technique, and thickness is not
Greater than 200 nanometers.
The matrix of the conductive gate layer is thermoplastic polyurethane, any one in Etheric ester type thermoplastic elastomer, covering
Flexible conducting material be carbon nanotube, silver nanowires, any one in copper nano-wire, density is not more than square resistance
1000 ohm.
The parallel strip-like electrodes layer uses silver or copper nano-wire as electrode conductive material, using inkjet printing methods system
It is standby to be taken in the pyramid item for being covered with carbon nanomaterial film layer, as single or fet structure of the parallel edge pricker bar with array
Source, leakage measuring electrode.
The method of the preparation quick sensing element of flexible force based on three-dimensional carbon nanomaterial fet structure, first prepares
Three-dimensional rib body bores layer, then prepares carbon nanomaterial film layer, then, prepares field in carbon nanomaterial thin-film surface with photoetching process
Pyramid strip portion photoetching process is first covered aqueous photoresist, then removes exposed portion with oxygen plasma by effect measurement area
Divide carbon nanomaterial film layer, then prepare silver or copper nano-wire electrode on pyramid band or band array with ink-jet printing,
Electrode line width is 40 to 150 microns, and the density of the nano line electrode remains square resistance not higher than 200 ohm, is adhered to
Source, drain electrode in carbon nanomaterial thin-film surface；One layer of Ionic colloid is deposited in above-mentioned carbon nanomaterial thin-film surface,
One layer of conductive gate layer is covered on above structure surface again, matrix is elastomeric material, and surface covers flexible conducting material, this is led
Electric layer lower surface is contacted with pyramid tips, forms removable field effect transistor gate；Wherein, when carbon nanomaterial film layer is
When continuous graphite alkene, copper surface three dimension rib body cone layer structure is prepared with template and electrodeposition process；Existed with chemical vapour deposition technique
Above-mentioned steel structure surface deposits single-layer or multi-layer graphene；It is filled in the minus of above-mentioned steel structure surface with elastomeric material, shape
At successive substrates thick film；Copper film is dissolved with aqueous solution, forms the graphene company for being covered on 3 d elastic body pyramidal structure surface
Continuous film；When carbon nanomaterial film layer is dispersing Nano carbon tubes, elastomer three-dimensional rib body cone layer structure is prepared with template；
Layer of semiconductor type single armed carbon nanotube is deposited in above-mentioned surface of elastomer with solution lacquering technique, the carbon nanotube for forming dispersion is thin
Film layer, thickness are not more than 10 nanometers；The carbon nanotube is prepared with chemical vapor deposition method, and 0.8 to 2.5 microns of length,
0.7 to 1.3 nanometers of diameter, electron mobility is not less than 102/ Vs, semi-conductor type carbon pipe content are greater than 95%, and dispersion liquid is first
Benzene.
Preparing copper surface three dimension rib body cone layer structure with template and electrodeposition process is first to prepare elastomer precursor gum with template
Film three-dimensional structure, step are as follows:
(5) single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then uses HF erosion removal
Oxide layer, then add isopropanol with tetramethyl aqueous ammonium hydroxide, corrode pyramid band etch pit minus out；
(6) mechanical after solidifying under vacuum with the above-mentioned pyramid-shaped silicon minus of the thermoplastic polyurethane filling heating of fusing
Removing, forms the polyurethane laminate of eurymeric；
(7) a strata methyl methacrylate is coated with lacquering technique on above-mentioned polyurethane eurymeric surface, thickness is micro- less than 1
The glue film that surface is covered with copper film after sufficiently dry, then with vacuum vapor deposition method is suspended on sulphur in one layer of fine copper of surface evaporation by rice
In sour copper electrolyte, using fine copper as anode, above-mentioned glue film eurymeric is cathode, slowly deposits one layer of fine copper on surface；
(8) after the copper film for finishing deposition cleans, is dry 1 minute in immersion toluene, taking-up drying, the removing of glue film eurymeric,
Copper film is continued after being impregnated 10 hours with chloroform, drying is taken out, is saved in dry pure nitrogen gas environment.
Single-layer or multi-layer graphene is deposited on steel structure surface with chemical vapor deposition method, specifically: by above-mentioned steel structure
It anneals 1 hour for 700 DEG C in hydrogen, is then discharged out hydrogen, be warming up to 900~1020 DEG C, kept for 1 hour, then is logical by 1:1 flow
Enter methane and hydrogen, is kept for 15 minutes at 900~1020 DEG C, then slow cooling, obtains the single layer or more for being grown in copper surface
Layer graphene.
The specific steps of elastomer three-dimensional rib body cone layer structure are prepared with template are as follows:
(1) single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then uses HF erosion removal
Oxide layer, then add isopropanol with tetramethyl aqueous ammonium hydroxide, corrode pyramid band etch pit silicon minus out；
(2) it is filled in the minus of above-mentioned silicon structure surface with elastomeric material, successive substrates thick film is formed, after vacuum solidification
Mechanical stripping forms elastomer glue film eurymeric.
The aqueous solution is iron chloride, ferric nitrate saturated solution.
Beneficial effect
The flexible force sensitive sensor of the method according to the invention preparation has the advantages that highly sensitive, high stability.The biography
Sensor sensitivity within the scope of 0 to 3MPa can be designed by structural adjustment, and maximum sensitivity can achieve 3MPa-1, tool
There are high-temperature, strain stable, minimum dimension can be wide to 20 microns, can be made into transparency higher than 80%, bending curvature less than 3 millis
The film power sensing structure of rice.
Detailed description of the invention
Fig. 1 is the quick sensing element preparation process schematic diagram of flexible force.
Fig. 2 is the quick sensing element pyramidal structure micro-image of typical structure flexible force.
Fig. 3 is the quick sensing element structural schematic diagram of flexible force.
Wherein, 1 is movable grid, and 2 be leakage, and 3 be gate bias, and 4 be source bias, and 5 be Ionic colloid.
Fig. 4 is load-field-effect conductance plots of typical element.
Specific embodiment
Graphene used in the present invention be with chemical vapor deposition in the single layer on three-dimensional copper pyramid minus surface or
Multi-layer graphene, the graphene form continuous covering to copper surface, and the uniformity of single-layer or multi-layer film is greater than 90%, the copper minus
Means of Electrodeposition, which is deposited on surface evaporation, to be had in the thermoplastic polyurethane eurymeric of one layer of copper, and the eurymeric is with after being filled in silicon minus
Stripping means preparation, silicon minus photoetching, caustic solution preparation, control corrosion rate condition, silicon rib on surface oxidation monocrystalline silicon piece
Cone cell minus surface roughness reaches bright grade, and pyramid tip radius of curvature is lower than 1 micron.
Carbon nanotube used in the present invention is semi-conductor type single-walled structure, is prepared using chemical vapor deposition method, length
0.8 to 2.5 microns, 0.7 to 1.3 nanometers of diameter, electron mobility is not less than 10cm2/ Vs, semi-conductor type carbon pipe content are
100%.
The graphene on copper pyramid band minus surface is transferred to by elastomer eurymeric surface using transfer method, then in chlorination
Copper substrate is dissolved in iron or ferric nitrate saturated aqueous solution, obtains shifting the continuous graphite alkene on elastomeric edges wimble structure surface.
Carbon nanotube is coated in elastomer eurymeric using lacquering technique, carbon nanotube layer thickness is not more than 10 nanometers.
The above-mentioned elastomeric edges wimble structure for being covered with graphene or carbon nanotube is gone with photoetching and oxygen plasma treatment
Then extra graphene or carbon nanotube in addition to measured zone prepare source, drain electrode parallel stripes with ink-jet printing again, i.e.,
In the measured zone including pyramid band by photoetching, development, the photoresist in protection region is obtained, develop exposure measurement zone
Part except domain removes the part graphene or carbon nanotube with oxygen plasma, then with ink-jet printing in vertical rib
Strip direction printing silver or copper nano-wire electrode are bored, density makes square resistance no more than 200 ohm, and width 40 to 150 is micro-
Rice is obtained using silver or copper nano-wire as source, the flexible structure of leakage measuring electrode.
Dielectric layer uses Ionic colloid, with lacquering technique in above-mentioned graphene or carbon nanotube and measuring electrode surface coating one
The mixing of layer 1- ethyl-3-methylimidazole double fluoroform semi-annular jade pendant imide salts ionic liquids and vinylidene fluoride-hexafluoropropylene copolymer
Object film, thickness are not more than 200 nanometers.Grid is greater than the elastomer thin film of pyramidal structure using hardness, sprays on its surface
Mist method coats one layer of carbon nanotube or silver nanowires or copper nano-wire, and density makes square resistance no more than 1000 ohm.
By the fixed voltage being applied on grid, the conductance on graphene or carbon nanotube band or band array is measured
Variation obtains the measurement to gate surface compressive load is applied to, and grid voltage is not more than 2 volts, and source, electric leakage interpolar measure voltage
No more than 1 volt.
The area and material that the load measurement range of above-mentioned sensing arrangement passes through design grid and pyramid interband support construction
Material is to adjust, and to the occasion for requiring sensor requirements transparent, using single pyramid band, width is lower than 40 microns, and use is lower
The grid conducting layer of density, available naked eyes can not differentiate, whole clearing degree be greater than 80% power sensing structure；It is small curved to requiring
The occasion of curvature, the grid of pyramid strip substrates and thickness less than 0.05 millimeter using thickness less than 0.1 millimeter, pyramid item
Band long side is parallel to bending direction, flexible sensing element of the available bending curvature less than 3 millimeters.The measurement spirit of above structure
Sensitivity can realize that effective pyramid width is at 20 microns to 150 microns by adjusting pyramid width.
Above structure measuring signal is microampere to the electric current of milliampere magnitude or sampling resistor is used to obtain a millivolt magnitude voltages
Signal is not necessarily to temperature-compensating, stone using the quick sensing element of the power of graphene since graphene has lower temperature specific conductance
The high flexibility of black alkene, carbon nanotube makes force sensing element have longer-term service life, by selection single band to multiple
Parallel stripes form array, can prepare the sensing unit of tens microns Dao several millimeters measurement areas.
The present invention discloses one kind based on the quick sensing element of flexible force of three-dimensional carbon nanomaterial fet structure and its preparation
Method；
Silicon face three-dimensional structure is prepared with template, which is 20 to 150 microns of bottom width of parallel one-dimensional pyramid band
Or array minus；
Copper surface three dimension structure, structure pyramid band identical with above-mentioned silicon structure are prepared with template and electrodeposition process
Or array minus；
Single-layer or multi-layer graphene is deposited on above-mentioned steel structure surface with chemical vapour deposition technique；
It is filled in the minus of above-mentioned steel structure surface with elastomeric material, forms successive substrates thick film；
Copper film is dissolved with aqueous solution, forms the graphene continuous film for being covered on 3 d elastic body pyramidal structure surface；
It is described to prepare coating semiconductor type carbon nano-tube elastomer three-dimensional rib body cone layer structure with template, it the steps include:
(1) single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then uses HF erosion removal
Oxide layer, then add isopropanol with tetramethyl aqueous ammonium hydroxide, corrode pyramid band etch pit minus out；
(2) it is filled in the minus of above-mentioned silicon structure surface with elastomeric material, formation successive substrates thick film, after mechanical stripping
Form elastomer eurymeric glue film；
(3) semiconductor type carbon nano-tube is coated in above-mentioned eurymeric film surface with lacquering technique, coating thickness is received no more than 10
Rice.
Prepare parallel strip-like electrodes in graphene or carbon nano tube surface with ink-jet printing, use silver or copper nano-wire as
Electrode conductive material, fet structure source, leakage measuring electrode as single or parallel edge pricker bar with array；
One layer of Ionic colloid dielectric material is deposited in above-mentioned graphene or carbon nano tube surface, forms dielectric layer；
One layer of conductive grid is covered on above structure surface, matrix is elastomeric material, and surface covers compliant conductive material
Material, the conductive layer lower surface are contacted with pyramid tips, form removable field effect transistor gate；
Compressive load is applied to gate upper surface and base film lower surface, applies constant voltage between grid and source and drain,
Curent change between measurement source and drain, obtains the source-drain current changed with compressive load, and it is quick to form highly sensitive flexible compression loading force
Sensing element；
When Ionic colloid dielectric material and relatively thin flexible conducting material, whole absorptivity is smaller than above structure
20%.
The preparation method of the copper surface three dimension structure, first prepares thermoplastic polyurethane three-dimensional structure with template,
Step are as follows:
(1) single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then uses HF erosion removal
Oxide layer, then add isopropanol with tetramethyl aqueous ammonium hydroxide, corrode pyramid band etch pit minus out；
(2) mechanical after solidifying under vacuum with the above-mentioned pyramid-shaped silicon minus of the thermoplastic polyurethane filling heating of fusing
Removing, forms the polyurethane laminate of eurymeric；
(3) a strata methyl methacrylate is coated with lacquering technique on above-mentioned polyurethane eurymeric surface, thickness is micro- less than 1
The glue film that surface is covered with copper film is suspended on sulphur after sufficiently dry, then with vacuum vapor deposition method one layer of fine copper of its surface evaporation by rice
In sour copper electrolyte, using fine copper as anode, above-mentioned glue film eurymeric is cathode, slowly deposits one layer of fine copper on surface；
(4) after the copper film for finishing deposition cleans, is dry 1 minute in immersion toluene, taking-up drying, the removing of glue film eurymeric,
Copper film is continued after being impregnated 10 hours with chloroform, drying is taken out, is saved in dry pure nitrogen gas environment.
It is described with chemical vapor-phase method steel structure surface deposit graphene, be by above-mentioned steel structure in hydrogen 700 DEG C move back
Fire 1 hour, is then discharged out hydrogen, is warming up to 900~1020 DEG C, is kept for 1 hour, then be passed through methane and hydrogen, In by 1:1 flow
900~1020 DEG C are kept for 15 minutes, and then slow cooling, obtains the single-layer or multi-layer graphene for being grown in copper surface.
Described to fill to form successive substrates thick film on above-mentioned steel structure surface with elastomeric material, elastomer is room temperature curing
Silicon rubber, thermoplastic polyurethane, any one in Etheric ester type thermoplastic elastomer (TPE)；
The aqueous solution dissolves copper film, and aqueous solution is iron chloride, iron nitrate solution saturated solution.
It is described to be used in graphene or carbon nano tube surface preparation field-effect measurement zone, first by pyramid strip portion photoetching process
Aqueous photoresist is covered, then removes expose portion graphene or carbon nanotube with oxygen plasma, then existed with ink-jet printing
Silver or copper nano-wire electrode are prepared on pyramid band or band array, electrode line width is 40 to 150 microns, the nano line electrode
Density remains square resistance not higher than 200 ohm, obtains the source, the drain electrode that are attached to graphene or carbon nano tube surface.
It is described deposit on the surface of graphene the double fluoroform semi-annular jade pendant imide salts ionic liquids of one layer of 1- ethyl-3-methylimidazole with
The mixture Ionic colloid dielectric film of vinylidene fluoride-hexafluoropropylene copolymer, is deposited on graphene or carbon with solution lacquering technique
Nanotube surface, thickness are not more than 200 nanometers.
The conductive grid, matrix are thermoplasticity polyurethane, any one in Etheric ester type thermoplastic elastomer, covering it is soft
Property conductive material be carbon nanotube, silver nanowires, copper nano-wire, density makes square resistance no more than 1000 ohm.
Embodiment one
It 1, is 500 nanometers in oxidated layer thickness with photoetching process, crystal orientation is micro- to prepare width 20 on the monocrystalline silicon piece of<100>
Rice is to 150 microns, 150 microns to 500 microns of length of single or multiple parallel photoresist windows, at hydrofluoric acid dissolution window
Then oxide layer is placed in the tetramethylammonium hydroxide aqueous solution and isopropyl alcohol mixture of 25% weight ratio of 1:1, at 95 DEG C
Lower corrosion, taking-up when cone cell tip is sufficiently formed obtain silicon pyramid minus after cleaning-drying；
2,2 millimeters of thickness of thermoplastic polyurethane thin slice is covered on silicon pyramid minus surface, is heated to 165 in a vacuum
DEG C, pressurization is kept for 5 minutes, is taken out, and peel-strength polyurethane glue-line after cooling and solidifying obtains polyurethane elastomer glue film eurymeric；
3, first by glue film eurymeric in molecular weight 996K, concentration is about that the polymethyl methacrylate chlorobenzene of 6% weight ratio is molten
It is impregnated in liquid, taking-up is 5 minutes dry at 150 DEG C, one layer of fine copper is deposited on its surface with vacuum vapor deposition method, thickness is greater than 100 and receives
Rice after drying is fixed, is placed in the bright electroplate liquid of bronzing, with glue film eurymeric then by its surface conductive adhesive electrode cable
For cathode, pure copper sheet is anode, deposits one layer of fine copper in silastic surface under constant voltage, thickness is not less than 1 millimeter；
4, it after being cleaned the copper film that deposition finishes with pure water, being dry, is placed in toluene, places 1 minute, the stripping of glue film eurymeric
From taking-up drying obtains copper minus, glue film can repeat step 3, be used to prepare another copper minus；
5, the copper minus of removing is impregnated 10 hours in chloroform, takes out drying, merging pure nitrogen gas environment saves；
6, graphene is deposited on copper minus surface with chemical vapour deposition technique, the steps include: copper minus in 0.6Pa hydrogen
In 700 DEG C anneal 1 hour, be then discharged out hydrogen, be warming up to 900~1020 DEG C, kept for 1 hour, then be passed through methane by 1:1 flow
And hydrogen, it is kept for 15 minutes at 900~1020 DEG C, then slow cooling, obtains the single-layer or multi-layer graphite for being grown in copper surface
Alkene.
7, the room curing silicon rubber liquid for being mixed with curing agent is added dropwise on the copper minus surface that growth has graphene, true
Aerial degasification after five minutes, is kept for 24 hours at room temperature, after silicon rubber sufficiently solidifies, then by the copper minus of filled silicon rubber
It is placed in the iron nitrate aqueous solution of saturation, places 24 hours, sufficiently dissolved to copper, take out silicon rubber, wash, is dry, obtaining table
Face is covered with the silicon rubber eurymeric of continuous graphite alkene；
8, the photoetching offset plate figure of covering pyramid measured zone is prepared with photoetching process, then removes exposed region with oxygen plasma
The graphene in domain, then band-like source, drain electrode are prepared in the pyramidal surface for being covered with graphene with ink-jet printing, by 0.5mg/ml
Copper nano-wire ethyl alcohol/glycolic suspension of concentration prints continuous parallel electricity in vertical pyramid strip direction with ink-jet printer
Pole, density make square resistance no more than 200 ohm, obtain using conducting nanowires as the field-effect source of electrode, drain electrode, will
Source, drain electrode extraction wire；
9, by the double fluoroform semi-annular jade pendant imide salts ionic liquids of 1- ethyl-3-methylimidazole of 10% weight ratio and inclined fluorine second
Alkene-hexafluoropropylene copolymer mixture (weight ratio 1:2) Ionic colloid dimethyl formamide solution is covered with lacquering technique in painting
Graphene and electrode surface are stated, it is 1 hour dry at 150 DEG C, Ionic colloid dielectric film is formed, thickness is not more than 200 nanometers；
10, with spray method thickness no more than 0.2 millimeter, hardness be 65A thermoplastic polyurethane film surface coated copper
Nano wire, spraying density make square resistance no more than 1000 ohm, and conducting surface is covered on step 8 by extraction wire after drying
Field effect element grid is formed above the pyramid band coated with ionic liquid of preparation, is encapsulated with silicon rubber, obtains overall thickness
The quick sensing element of flexible force less than 1 millimeter；
11, apply constant 1 volt of positive voltage on grid, depending on measurement area size and band number, applied in source, electric leakage interpolar
Add 0.1 to 1 volt positive voltage, electric current obtains sensing element with the variation for being applied to gate upper surface compressive load between measurement source, leakage
Standard calibration curve, obtain obtaining to unknown Load Sensitive range is endogenous, the corresponding load of leakage current with this calibration curve
The measurement of load.
Embodiment two
1, as in the first embodiment, 1；
2, as in the first embodiment, 2；
3, layer of semiconductor type carbon nanotube, carbon nanotube dispersion are coated in polyurethane elastomer glue film eurymeric with lacquering technique
In toluene solution, concentration 0.02mg/ml is not more than 10 nanometers in the carbon nano-tube film thickness of pyramidal surface dispersion, In
It is 1 hour dry at 140 DEG C；
4, as in the first embodiment, 8；
5, as in the first embodiment, 9；
6, as in the first embodiment, 10；
7, as in the first embodiment, 11.
Claims (5)
1. a kind of method for preparing the quick sensing element of flexible force based on three-dimensional carbon nanomaterial fet structure, it is characterized in that:
Three-dimensional rib body cone film layer is first prepared, then prepares carbon nanomaterial film layer, then, with photoetching process in carbon nanomaterial film layer table
Pyramid strip portion photoetching process is first covered aqueous photoresist, is then gone with oxygen plasma by wheat flour for field-effect measurement zone
Except expose portion carbon nanomaterial film layer, then silver or copper nano-wire electricity are prepared on pyramid band or array with ink-jet printing
Pole, electrode line width are 40 to 150 microns, and the density of the nano line electrode remains square resistance not higher than 200 ohm, are obtained attached
The source in carbon nanomaterial thin-film surface, drain electrode；The sub- glue of a leafing is deposited in above-mentioned carbon nanomaterial thin-film surface
Body is prepared pyramidal layer, then covers one layer of conductive gate layer in above-mentioned pyramidal layer body structure surface, and the matrix of conductive gate layer is
Elastomeric material, surface cover flexible conducting material, which contacts with pyramid tips, form removable field
Effect transistor grid；Wherein, when carbon nanomaterial film layer is continuous graphite alkene, copper is prepared with template and electrodeposition process
Surface three dimension rib body bores film layer structure；Single-layer or multi-layer graphene is deposited on copper surface with chemical vapour deposition technique；Use elastomer
Material is filled in the minus of copper surface, forms successive substrates thick film；Copper film is dissolved with aqueous solution, formation is covered on three dimensional elasticity
The graphene continuous film on body pyramidal structure surface；When carbon nanomaterial film layer is dispersing Nano carbon tubes, with template legal system
Standby elastomer three-dimensional rib body bores film layer structure；Layer of semiconductor type single armed carbon is deposited in above-mentioned surface of elastomer with solution lacquering technique
Nanotube, forms the carbon nano-tube film layer of dispersion, and thickness is not more than 10 nanometers；The carbon nanotube chemical vapor deposition
Method preparation, 0.8 to 2.5 microns of length, 0.7 to 1.3 nanometers of diameter, electron mobility is not less than 102/ Vs, semi-conductor type carbon
Pipe content is greater than 95%, and dispersion liquid is toluene；
The obtained quick sensing element of flexible force based on three-dimensional carbon nanomaterial fet structure by centrum layer and is covered on centrum
Conductive gate layer on layer is constituted；The centrum layer is followed successively by elastomer three-dimensional rib body cone film layer, carbon nanometer by center outward
Material film layers, parallel strip-like electrodes layer, Ionic colloid dielectric materials layer；The elastomer three-dimensional rib body cone film layer is several
Three-dimensional rib body taper at parallel one-dimensional pyramid band or array, 20-150 microns of bottom width of the described three-dimensional rib body cone；It is described
Conductive gate layer matrix be elastomeric material, surface cover flexible conducting material, conductive material layer and centrum layer three-dimensional
The tip contact of rib body cone forms removable field effect transistor gate；The carbon nanomaterial film layer is continuous graphite
Alkene or dispersing Nano carbon tubes.
2. the method as described in claim 1, it is characterized in that: preparing copper surface three dimension rib body cone film with template and electrodeposition process
Layer structure is first to prepare elastomer glue film three-dimensional structure, step with template are as follows:
Single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then use HF erosion removal oxide layer,
Add isopropanol with tetramethyl aqueous ammonium hydroxide again, corrodes pyramid band etch pit minus out；
With the pyramid band etch pit minus of the thermoplastic polyurethane filling heating of fusing, mechanical stripping after solidifying under vacuum,
Form the polyurethane laminate of eurymeric；
Above-mentioned eurymeric polyurethane adhesive film surface with lacquering technique coat a strata methyl methacrylate, thickness less than 1 micron,
After sufficiently dry, then with vacuum vapor deposition method the glue film that surface is covered with copper film is suspended on sulfuric acid in one layer of fine copper of surface evaporation
In copper electrolyte, using fine copper as anode, above-mentioned glue film is cathode, slowly deposits one layer of fine copper on surface；
After the copper film that deposition is finished cleans, is dry 1 minute in immersion toluene, drying is taken out, glue film removing continues copper film
After being impregnated 10 hours with chloroform, drying is taken out, is saved in dry pure nitrogen gas environment.
3. the method as described in claim 1, it is characterized in that: depositing single-layer or multi-layer stone on copper surface with chemical vapour deposition technique
Black alkene, specifically: by copper surface, 700oC anneals 1 hour in hydrogen, is then discharged out hydrogen, is warming up to 900 ~ 1020oC, keeps
1 hour, then it is passed through methane and hydrogen by 1:1 flow, it is kept for 15 minutes in 900 ~ 1020oC, then slow cooling, is grown
Single-layer or multi-layer graphene on copper surface.
4. the method as described in claim 1, it is characterized in that: preparing the tool of elastomer three-dimensional rib body cone film layer structure with template
Body step are as follows:
Single or multiple ribbon windows first are made by lithography in the silicon chip surface for having oxide layer, then use HF erosion removal oxide layer,
Add isopropanol with tetramethyl aqueous ammonium hydroxide again, corrodes pyramid band etch pit silicon minus out；
It is filled in pyramid band etch pit silicon minus with elastomeric material, forms successive substrates thick film, it is mechanical after vacuum solidification
Removing forms elastomer glue film eurymeric.
5. the method as described in claim 1, it is characterized in that: the aqueous solution is iron chloride, ferric nitrate saturated solution.
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| CN111693189B (en) * | 2020-05-29 | 2022-04-15 | 南京邮电大学 | Novel flexible force-sensitive sensor and preparation method thereof |
| CN113155329A (en) * | 2021-02-05 | 2021-07-23 | 宝峰时尚国际控股有限公司 | Pressure sensor and preparation method thereof |
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