CN106768513B - A kind of pressure sensor and preparation method thereof - Google Patents

A kind of pressure sensor and preparation method thereof Download PDF

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CN106768513B
CN106768513B CN201611079246.8A CN201611079246A CN106768513B CN 106768513 B CN106768513 B CN 106768513B CN 201611079246 A CN201611079246 A CN 201611079246A CN 106768513 B CN106768513 B CN 106768513B
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graphite
graphite material
preparation
pressure
pressure sensor
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CN106768513A (en
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王紫东
彭沛
田仲政
任黎明
傅云义
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Peking University
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Peking University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/18Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material

Abstract

The invention discloses a kind of simple wide range of structure and high-precision pressure sensors and preparation method thereof.There are the nano thickness graphite materials of a large amount of folds using surface for this method, electric conductivity based on fold in a direction orthogonal to the surface can significantly increase this phenomenon with the increase for the pressure born on fold, devise the pressure sensor structure that a structure is simple, is easily achieved.Since the fold on graphite material surface is ubiquitous, density is larger, and height is different, so the pressure sensor can not only realize the measurement to pressure in biggish range ability, but also also very high to the precision of pressure measurement, the measurement to micro- power may be implemented.In addition, the pressure sensor also has advantage small in size since graphite material is nano thickness laminated structure.

Description

A kind of pressure sensor and preparation method thereof
Technical field
The invention belongs to art of pressure sensors, and in particular to a kind of simple wide range of structure and high-precision pressure pass The preparation method of sensor.
Background technique
Pressure sensor refers to that by pressure conversion be the device that can survey electric signal.Pressure sensor is very widely used, The industrial requirements such as automated system are applied to, from the accurate measurement of micro- power such as precision balance to general from scientific explorations such as wind-force measurements The general object check weighing such as logical electronic balance, suffers from indispensable role in every field.And for different fields, it is required Required precision, range ability of the pressure of measurement etc. are often different, therefore according to different pressure measurement demands, are used Pressure capsule system (including stressing device, pressure sensor, conversion element etc.) all there are great differences.
The measurement of power micro- for such as precision balance etc. mainly uses laser displacement formula, photo-electric, condenser type and electromagnetic force The sensors such as formula need to generally cooperate facula position detection amplification system, photoelectric amplification system or electricity as pressure sensing component Differential amplification system etc. amplifies come the signal exported to pressure sensor, and check weighing range is mainly 10-5~103G (is pressed The pressure limit that force snesor is perceived is 10-7~10N);For the check weighing of general object, ordinary electronic balance is mainly used, Its pressure sensor is generally the pressure sensor of resistance-strain type, and precision is relatively poor, and check weighing range is generally 10-1~ 105(pressure limit that i.e. pressure sensor is perceived is 10 to the range of g-3~103N).In general, the biggish pressure of measuring range Force snesor precision is poor;And the higher pressure sensor of precision is unable to measure biggish pressure.In addition, these pressure sensors Need to carry out it is well-designed, to realize pressure sensing function, and with the other component in pressure-measuring system (as detected electricity Road, signal processing unit etc.) it is compatible, therefore structure is often more complicated.
Summary of the invention
It is an object of the invention to design a kind of simple wide range of structure and high-precision pressure sensor, main work Make principle are as follows: (average thickness of the graphite material is 10~500nm, below there are the graphite material of a large amount of folds for surface Abbreviation graphite), when use conduction mode atomic force microscope (c-AFM) carries out longitudinal conductivity measurement (i.e. in stone on its surface Black surface applies the voltage in its normal direction, and the differential conductance in this direction of survey calculation) Shi Faxian, the differential at fold The conductance of conductance ratio flat place is much bigger.Moreover, when probe is applied to the pressure on fold and constantly increases, due to being sent out at fold Increasing deformation is given birth to, longitudinal differential conductance of the same measurement point can be continuously increased, and eventually arrive at a saturation value, such as Fig. 1.Therefore, if indicating the pressure of graphite fold receiving with longitudinal differential conductance of graphite fold, there are a large amount of pleats on surface The graphite of wrinkle can be used as a simple pressure sensor of structure.
The present invention provide pressure sensor include-surface there are the graphite material of fold, which is nano thickness Laminated structure;The graphite material is adhered to the intermediate region of a piece of hard metal on piece;Another hard metal piece is covered on On graphite material, the edge of above-mentioned two panels hard metal piece using flexible insulating material adhesion and is encapsulated, and preparation method includes Key step it is as follows:
1) there are the graphite material of fold, which is nano thickness laminated structure on preparation surface;
Above-mentioned graphite material refers to that average thickness is the nano thickness graphite material of 10~500nm.
Above-mentioned graphite material refers to the graphite material prepared by chemical vapour deposition technique (CVD).
When preparing graphite, if the base material of preparation is metal, which can not have to removal;And if system Standby base material is insulating materials or the poor material of electric conductivity, then the substrate needs to remove.
2) minimum area and maximum area of graphite material needed for calculating, and according to this calculated result, it is suitable in graphite Region cut out the graphite material of certain area;
Since longitudinal differential conductance of graphite has saturation value, so to calculate the minimum area S of required graphite materialG1.Benefit Topography measurement is carried out to graphite surface with atomic force microscope (AFM), and according to the different purposes of pressure sensor, needed for determining The range ability of the power of measurement, thus the area minimum area S of graphite material required for calculatingG1, calculation method are as follows:
A. using the shape appearance figure of AFM measurement graphite upper surface (i.e. the one side of surface folding protrusion), such as Fig. 2.According to the shape Looks figure, calculate the area of fold on graphite: for the convenience of calculating, the area of fold is quantified as a rectangle, and width is with pleat The halfwidth of wrinkle calculates, and length directly measures on shape appearance figure, and the gross area that fold is calculated is SW.And entire shape appearance figure is Square, side length can be directly read from figure, be denoted as L, then the area of entire scanning area graphite is L2.In order to accurate Reflection fold accounts for the percentage of entire graphite material, and the region of scanning is unsuitable too small (L >=10 μm);But in order to reduce fold The amount of calculation of area, scanning area also should not be too large (L≤30 μm).
B. in general, fold width far more than needle point diameter, it is believed that the area of AFM probe needle point be needle point with The contact area of graphite fold, is denoted as ST.For conduction mode AFM probe, needle point area is about 1200nm2
C. and according to the relationship of pressure in Fig. 1 and differential conductance, when the pressure that needle point applies is greater than 40nN, the electricity of fold It leads and is up to saturation value, at this moment fold will lose the measurement capability of power.Therefore, in order to be accurately realized the measurement of power, needle point Pressure is no more than a fixed value FT, this value is generally 10-8The magnitude of N.
D. therefore, the maximum value of the pressure if desired measured is FM, then needed for graphite minimum area SG1Can according to Lower formula is calculated:Wherein, ST=1200nm2, FT=10-8N。
In addition, also to calculate the maximum area S of required graphite materialG2, this is because: AFM is to graphite surface according to fig. 2 The characterization result of pattern, it can be seen that the height of each fold of graphite surface is different, some crimp height is higher, Some crimp height is lower.When the pressure of application is lesser, miniature deformation, lower pleat occur for only high fold Any deformation does not occur for wrinkle, the precise measurement that the fold of this sub-fraction deformation will make pressure sensor realize micro- power.Also It is to say, in order to realize the precise measurement of micro- power, the total quantity of higher fold should not be excessive in used graphite, because This, the maximum area S of used graphiteG2It should meet: SG2=10 × SG1
When being characterized to graphite upper surface topography, the atomic force microscope mode used can be common contact mode, Common tapping-mode, conduction mode, electrostatic force mode, magnetic mode, Kelvin Force mode, peak value force mode or automatic mode Deng.
No matter using the preparation of which kind of method graphite material, all there is impurity, broken hole and in uneven thickness etc. in surface Problem.Therefore, it is necessary to select graphite regions use clean, that thickness is uniform on graphite, to guarantee made pressure sensing Power suffered by device is uniformly and stably dispersed in each region of graphite material.
The small pieces graphite cut needs to be free of broken hole or broken hole area regular shape that is smaller, but also need to cutting, with Just the gross area S of graphite can be calculatedG.The method of cutting can be directly to be cut using macro tools such as scissors, pocket knives, It is also possible to micro- using ultraviolet photolithographic, electron beam exposure, laser direct-write photoetching, nano-imprint lithography or focused-ion-beam lithography etc. Machining tool is processed.
3) graphite material cut out is adhered to the intermediate region of a piece of hard metal on piece using conducting resinl;
The conducting resinl used answers it to have stronger conductive capability, and can guarantee the lower surface of graphite and hard metal piece have compared with Big contact area can be conductive silver glue, sliver-powder conducting glue, carbonaceous conductive adhesive tape, cupric powder conductive adhesive, copper conductive adhesive band, graphite Filled conductive glue etc..
4) another hard metal piece is covered in the another side of graphite material, which relies on the upper table of gravity and nickel foil Face contacts naturally, and the edge of two panels hard metal piece uses flexible insulating material adhesion, and entire pressure sensor is linked as one Body, and realize encapsulation;
Before covering hard metal piece, need to coat a circle flexible insulating material, such as Fig. 3 along the edge of sheet metal. Then, another piece of hard metal piece is covered to the upper surface of graphite.This block hard metal piece, both can be with due to gravity Fold on graphite is close to, and can pass through the metal of the flexible insulating material and lower surface after flexible insulating material solidification Piece forms adherency, the schematic diagram of the pressure sensor such as Fig. 4.Two hard metal pieces of graphite surface covering, are similar to two Electrode can be measured perpendicular to the electric current on graphite direction when applying fixed voltage on two sheet metals with pressure Variation, to calculate the variation of corresponding differential conductance.
Used hard metal piece can be the metal simple-substance of all types or the alloy cpd of each metalloid.
The metal material that can be same type for two hard metal pieces of covering, is also possible to different types of gold Belong to material, but is both needed to bigger than the area of the graphite material used so that it is convenient to coat a circle flexible insulation material on sheet metal Material.
Used flexible insulating material should have stronger viscosity, stronger flexible, preferable insulating properties and compared with Good leakproofness, can be dimethyl silicone polymer (PDMS), polymethyl methacrylate (PMMA), poly terephthalic acid second two Alcohol ester (PET), polyethylene naphthalate (PEN), polytetrafluoroethylene (PTFE) (PTFE), polyimides (PI), polycarbonate (PC), Polyvinyl chloride (PVC), cellulose acetate (CA), polytrifluorochloroethylene (PCTFE) etc..Wherein, stronger viscosity can guarantee two Sheet metal adheres to firm;Stronger flexibility is the true measurement in order to preferably realize pressure;Preferable insulation performance guarantees Between two sheet metals conductive path must be formed by graphite;The good of the pressure sensor may be implemented in preferable leakproofness Good encapsulation.
5) pressure sensor is linked into respective measurement system, the pressure is passed to be realized in the measuring system The calibration of sensor.
In the pressure sensor, have many factor can interference measurement results authenticity, it is hard such as graphite upper surface The internal resistance that the gravity of matter sheet metal, the flexible material used introduce the support force and sheet metal and conductive silver glue of sheet metal Deng, it is therefore desirable to differential conductance value when not applying pressure is measured and calculated, and this value is set as to the zero point of pressure.
In order to read the pressure value measured, it is also necessary to using the counterweight of different quality, read each counterweight to pressure When sensor applies different pressures, corresponding differential conductance value, and be fitted.In this way, often measuring a differential conductance value, just A specific pressure value can be corresponded to, to realize pressure sensing function.
Technical characterstic of the invention: there are the nano thickness graphite materials of a large amount of folds on surface, perpendicular to its surface side Upward electric conductivity can be significantly increased with the increase for the pressure born on surface folding.The physical principle letter of this phenomenon It is single, thus it is very simple using the pressure sensor structure that the graphite is designed, and easily realize.Because fold is in graphite material table Face is ubiquitous, and density is generally large, therefore the range of power that the pressure sensor can measure is often larger, i.e. range It is larger.Again since the crimp height of graphite surface has a certain difference, when pressure is smaller, only higher a part The detection to micro- power may be implemented when the fold of stress is less in fold stress, therefore the precision of the pressure sensor is also very It is high.In addition, the pressure sensor also has advantage small in size since graphite material is nano thickness laminated structure.
Detailed description of the invention
Fig. 1 is bent using the relationship of the c-AFM longitudinal differential conductance measured at a fold on graphite and fold stress Line;
The graphite surface shape appearance figure that Fig. 2 is measured using AFM;
Fig. 3 not on graphite material cover hard metal piece when pressure sensor schematic diagram;
The complete structure sectional view of Fig. 4 pressure sensor;
1-graphite material in figure;The fold on 2-graphite material surfaces;3-hard metal pieces;4-conducting resinls;5-is flexible Insulating materials.
Specific embodiment
Below by example, the present invention will be further described.It should be noted that the purpose for publicizing and implementing example is to help It helps and further understands the present invention, but it will be appreciated by those skilled in the art that: do not departing from the present invention and appended claims Spirit and scope in, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to interior disclosed in embodiment Hold, the scope of protection of present invention is subject to the scope defined in the claims.
Example 1: applied to the pressure sensor in precision balance.
1) in the appropriate area of the graphite of CVD method preparation, common tapping-mode (the probe model OTESPA- of AFM is used R3 topography measurement) is carried out to graphite surface.
According to the shape appearance figure that measurement obtains, the side length L of shape appearance figure is 10 μm, and the fold in the calculated shape appearance figure is total Area SWAbout 50 μm2.For general precision balance, the maximum value F for the pressure for needing to measureMGenerally 10N.Will more than Data substitute into formulaIn, the minimum area S of required graphite can be calculatedG1It is 2.4 × 10-6m2
Precision balance needs the higher pressure sensor of service precision, therefore the area of selected graphite material is not low It is small as far as possible under the requirement of minimum area, while to guarantee to meet the needs of range, realize high-acruracy survey.
2) it calculates for convenience, the suitable region on graphite, cuts out the square graphite regions that side length is 2mm;
The square graphite for the use of a piece of side length being 1cm, uses its surface topography of optical microphotograph sem observation, it is ensured that entire stone Graphite on ink sheet is clean, thickness is uniform and without broken hole.Then the method for using uv-exposure, meets paracentral area on graphite flake Domain exposes the square area that a side length is 2mm out, and the graphite of rest part is fallen using oxygen plasma etch.Exposure finishes Afterwards, using the acetone soak graphite flake, to remove the photoresist on surface.After removing photoresist, absolute alcohol and deionized water are successively used It cleans, and dries up.
3) taking a piece of diameter is the round hard copper sheet of 3cm, and it is about 1cm that area is coated in region therebetween2Conductive silver Glue, conductive silver glue covering region should approximation be square, the graphite material cut out is then adhered to the hard at once The region (hard copper on piece post graphite material be denoted as front on one side) of conductive silver glue is coated on copper sheet.Then by the hard copper Piece face-up stands 30 minutes, spontaneously dries to conductive silver glue.
4) at the positive proximal edge of hard copper sheet, upper circle PMMA glue is dripped, drips the track of glue as far as possible close to round hard The edge of copper sheet.Another hard copper sheet is covered in the another side of the graphite material later, and stands 2min, to guarantee covering Hard copper sheet is close to graphite material.Pressure sensor will finally be carried out as, with 120 DEG C of baking 30min, making PMMA on hot plate Solidification.
5) make pressure sensor one side fixed, another side is connected on an insulation bearing tray, and by two hard coppers Piece is connect with the positive and negative anodes of a precision ammeter.Then, measure respectively and calculate unloaded and pallet plus 100ug, 1mg, 10mg ... the corresponding differential conductance value of each weight after the counterweights such as 100g, 1000g, and be fitted using computer, thus Complete the calibration to the pressure sensor.
Example 2: the pressure sensor applied to ordinary electronic scale.
1) in the appropriate area of the graphite of CVD method preparation, the common contact mode (probe model SNL-10) of AFM is used Topography measurement is carried out to graphite surface.
According to the shape appearance figure that measurement obtains, the side length L of shape appearance figure is 20 μm, and the fold in the calculated shape appearance figure is total Area SWAbout 80 μm2.For general ordinary electronic scale, the maximum value F for the pressure for needing to measureMGenerally 500N.It will be with Upper data substitute into formulaIn, the minimum area S of required graphite can be calculatedG1It is 4 × 10-4m2
2) it calculates for convenience, the suitable region on graphite, cuts out the square graphite regions that side length is 2cm;
Using optical microscopy, which is observed, and the selection of its surface is clean, thickness is uniform and without broken The region in hole, is cut out using pocket knife, finally obtains the square area that a side length is 2cm.
3) taking a piece of diameter is the round hard copper sheet of 5cm, and it is about 2.5cm's that one piece of side length is sticked in region therebetween Then the graphite material cut out is adhered to the region that conductive copper glue is posted on the hard copper sheet surface by square conductive copper glue (hard copper on piece post graphite material be denoted as front on one side).
4) at the positive proximal edge of hard copper sheet, upper circle PDMS is dripped, drips the track of glue as far as possible close to round hard copper The edge of piece.Another hard copper sheet is covered in the another side of the graphite material later, and stands 2min, to guarantee the hard of covering Matter copper sheet is close to graphite material.It is solidifying as PDMS with 125 DEG C of baking 20min, is made on hot plate that pressure sensor will finally be carried out Gu.
5) make pressure sensor one side fixed, another side is connected on an insulation bearing tray, and by two hard coppers Piece is connect with the positive and negative anodes of a precision ammeter.Then, measure respectively and calculate unloaded and pallet plus 0.5g, 5g, 50g ... the corresponding differential conductance value of each weight after the counterweights such as 5kg, and be fitted using computer, to realize to the pressure The calibration of sensor.
Example 3: the pressure sensor applied to electronic product.
1) people more or less can apply it certain when touching the touch screen and touch tablet of common electronic products Pressure, the range of general pressure is 10-2Change between~1N.And general electronic products use the common screen and common of touching Touch tablet can not identify the size of pressure although they can respond touch operation.Commonly to touch screen and common The small-sized electronic products such as touch tablet realize the response to pressure, it is necessary to cooperate relatively thin, more accurate pressure sensor.So choosing The graphite material containing more fold for taking CVD method to prepare, and it is right with the common contact mode of AFM (probe model SNL-10) Graphite surface carries out topography measurement.
According to the shape appearance figure that measurement obtains, the side length L of shape appearance figure is 20 μm, and the fold in the calculated shape appearance figure is total Area SWAbout 80 μm2.Common people touch the pressure of screen generally 10-2In the range of~1N.Above data is substituted into formulaIn, the minimum area S of required graphite can be calculatedG1It is 6 × 10-7m2
2) it calculates for convenience, the suitable region on graphite, cuts out the square graphite regions that side length is 1mm;
The square graphite flake for the use of a piece of side length being 1cm, uses their surface topography of optical microphotograph sem observation, it is ensured that Graphite on the graphite flake is clean, thickness is uniform and without broken hole.Then the method for using uv-exposure, close to center on graphite flake Regional exposure go out the square area that a side length is 1mm, the graphite of rest part fallen using oxygen plasma etch.Exposure After, using the acetone soak graphite flake, to remove the photoresist on surface.After removing photoresist, successively using absolute alcohol and go from Sub- water is cleaned, and is dried up.
3) the thin hard copper sheet of square that a piece of side length is 2cm is taken, and is applied above in the intermediate region of the thin hard copper sheet Product is about 1cm2Conductive silver glue, conductive silver glue covering region should approximation be square, the graphite that then will be cut out at once Material is adhered to the thin hard copper on piece and is coated with the region of conductive silver glue (hard copper on piece posts being denoted as on one side just for graphite material Face).Then the hard copper sheet is face-up stood 30 minutes, is spontaneously dried to conductive silver glue.
4) at the positive proximal edge of thin hard copper sheet, the suitable PDMS of a upper circle is dripped, drips the track of glue as far as possible close to just The edge of rectangular thin hard copper sheet.Another hard scale copper is covered in the another side of graphite material later, and stands 2min, with Guarantee that the hard scale copper of these coverings is close to graphite material.To finally carry out pressure sensor as on hot plate with 125 DEG C 20min is toasted, PDMS is solidified.
5) pressure sensor is corrected: timing, two hard scale coppers of pressure sensor respectively with one The positive and negative anodes of precision ammeter connect.Then, measure and calculate respectively zero load and on hard scale copper apply 0.01N, The corresponding differential conductance value of the power such as 0.1N, 1N, and be fitted using computer, to complete the school to the pressure sensor It is quasi-.
Although the present invention has been disclosed in the preferred embodiments as above, however, it is not intended to limit the invention.It is any to be familiar with ability The technical staff in domain, without departing from the scope of the technical proposal of the invention, all using in the methods and techniques of the disclosure above Appearance makes many possible changes and modifications or equivalent example modified to equivalent change to technical solution of the present invention.Therefore, Anything that does not depart from the technical scheme of the invention are made to the above embodiment any simple according to the technical essence of the invention Modification, equivalent variations and modification, all of which are still within the scope of protection of the technical scheme of the invention.

Claims (10)

1. a kind of pressure sensor, which is characterized in that including-surface there are the graphite material of fold, which is nanometer Thickness laminated structure;The graphite material is adhered to the intermediate region of a piece of hard metal on piece;Another hard metal piece covers It covers on graphite material, the edge of two panels hard metal piece using flexible insulating material adhesion and encapsulates, and passes perpendicular to pressure Electric conductivity on sensor surfaces direction can be significantly increased with the increase for the pressure born on graphite material surface folding.
2. a kind of preparation method of pressure sensor, comprises the following steps:
1) there are the graphite material of fold, which is nano thickness laminated structure on preparation surface;
2) topography measurement, selection cleaning, the uniform region of thickness, according to pressure are carried out to graphite material surface using atomic force microscope The range ability of measuring force needed for force snesor cuts graphite material;
3) above-mentioned graphite material is adhered to the intermediate region of a piece of hard metal on piece using conducting resinl;
4) another hard metal piece is covered on the another side of graphite material, the edge of two panels hard metal piece uses flexible Insulating materials adhesion simultaneously encapsulates, and forms pressure sensor as described in claim 1;
5) pressure sensor is linked into respective measurement system, and school is carried out to the pressure sensor in the measuring system It is quasi-.
3. preparation method as claimed in claim 2, which is characterized in that the average thickness of graphite material described in step 1) is 10 ~500nm.
4. preparation method as claimed in claim 2, which is characterized in that graphite material described in step 1) is to use chemical gaseous phase The graphite material of sedimentation CVD preparation.
5. preparation method as claimed in claim 2, which is characterized in that the measurement mould of atomic force microscope described in step 2) Formula is common contact mode, common tapping-mode, conduction mode, electrostatic force mode, magnetic mode, Kelvin Force mode, peak value Force mode or automatic mode.
6. preparation method as claimed in claim 2, which is characterized in that conducting resinl described in step 3) is conductive silver glue, silver Powder conducting resinl, carbonaceous conductive adhesive tape, cupric powder conductive adhesive, copper conductive adhesive band, graphite-filled type conducting resinl or other with excellent conductive The glue of ability.
7. preparation method as claimed in claim 2, which is characterized in that the method for cutting described in step 2) is scissors or small The direct cutting or ultraviolet photolithographic, electron beam exposure, laser direct-write photoetching, nano-imprint lithography or focused ion beam that knife carries out Etch the processing carried out.
8. preparation method as claimed in claim 2, which is characterized in that hard metal piece described in step 3) and step 4) is Refer to the metal simple-substance of all types or the alloy cpd of each metalloid.
9. preparation method as claimed in claim 2, which is characterized in that flexible insulating material described in step 4) refers to poly- two Methylsiloxane, polymethyl methacrylate, polyethylene terephthalate, polyethylene naphthalate, polytetrafluoroethyl-ne Alkene, polyimides, polycarbonate, polyvinyl chloride, cellulose acetate, polytrifluorochloroethylene.
10. preparation method as claimed in claim 2, which is characterized in that calibration described in step 5) refers to corresponding measurement The correction of system progress zero correction and corresponding scale division value corresponding pressure value.
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