CN106768513A - 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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Publication number
CN106768513A
CN106768513A CN201611079246.8A CN201611079246A CN106768513A CN 106768513 A CN106768513 A CN 106768513A CN 201611079246 A CN201611079246 A CN 201611079246A CN 106768513 A CN106768513 A CN 106768513A
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graphite material
graphite
pressure sensor
preparation
pressure
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CN106768513B (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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    • 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

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  • General Physics & Mathematics (AREA)
  • Measuring Fluid Pressure (AREA)

Abstract

Wide range and high-precision pressure sensor the invention discloses a kind of simple structure and preparation method thereof.There is the nano thickness graphite material of a large amount of folds using surface in the method, this phenomenon can be significantly increased with the increase of the pressure born on fold based on fold electric conductivity in a direction orthogonal to the surface, the pressure sensor structure for devise a simple structure, being easily achieved.Because the fold on graphite material surface is ubiquitous, density is larger, and it is highly different, so the pressure sensor can not only realize the measurement to pressure in the range of larger quantities journey, and it is also very high to the precision of pressure measxurement, it is possible to achieve the measurement to micro- power.Further, since graphite material is nano thickness laminated structure, the pressure sensor also advantage with small volume.

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 wide range of simple structure and high-precision pressure are passed The preparation method of sensor.
Background technology
Pressure sensor, it by pressure conversion is the device that can survey electric signal to refer to.The application of pressure sensor widely, Be applied to the industrial requirements such as automated system from scientific explorations such as wind-force measurements, from the accurate measurement of micro- power such as precision balance to general The general object check weighing such as logical electronic balance, indispensable effect is suffered from 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 measxurement demands, are used Pressure capsule system (including stressing device, pressure sensor, conversion element etc.) all exist very big difference.
It is main to use laser displacement formula, photo-electric, condenser type and electromagnetic force for the measurement of micro- power such as such as precision balance The sensors such as formula need to typically coordinate facula position to detect amplification system, photoelectric amplification system or electricity as pressure sensing component Differential amplification system etc. is amplified to the signal that pressure sensor is exported, and its check weighing scope is main 10-5~103G (is pressed The pressure limit that force snesor is perceived is 10-7~10N);It is main to use ordinary electronic balance for the check weighing of general object, Its pressure sensor is generally the pressure sensor of resistance-strain type, and precision is relatively poor, and its check weighing scope is general 10-1~ 105(pressure limit that i.e. pressure sensor is perceived is 10 to the scope of g-3~103N).In general, the larger pressure of measurement range Force snesor precision is poor;And precision pressure sensor higher cannot measure larger pressure.In addition, these pressure sensors Need to carry out it is well-designed, to realize pressure sensing function, and with pressure-measuring system in miscellaneous part (as detected electricity Road, signal processing unit etc.) it is compatible, therefore structure is often more complicated.
The content of the invention
Wide range and high-precision pressure sensor it is an object of the invention to design a kind of simple structure, its main work It is as principle:For surface exist a large amount of folds graphite material (average thickness of the graphite material be 10~500nm, below Abbreviation graphite), when carrying out longitudinal conductivity measurement (i.e. in stone on its surface using conduction mode AFM (c-AFM) Black surface applies the voltage in its normal direction, and this direction of survey calculation differential conductance) when find, the differential at fold The conductance of conductance ratio flat place is much bigger.And, when the pressure that probe is applied on fold constantly increases, due to being sent out at fold Increasing deformation is given birth to, longitudinal differential conductance of same measurement point can be continuously increased, and eventually arrive at a saturation value, such as Fig. 1.Therefore, if representing the pressure that graphite fold bears with longitudinal differential conductance of graphite fold, there are a large amount of pleats in surface The graphite of wrinkle just can be used as a pressure sensor for simple structure.
The present invention provide pressure sensor include-there is the graphite material of fold in surface, the graphite material is nano thickness Laminated structure;The graphite material sticks to the zone line on a piece of hard metal piece;Another hard metal piece is covered in On graphite material, above-mentioned two panels hard metal piece edge is using flexible insulating material adhesion and encapsulates, its preparation method is included Key step it is as follows:
1) graphite material that surface has fold is prepared, the graphite material is nano thickness laminated structure;
Above-mentioned graphite material refers to the nano thickness graphite material that average thickness is 10~500nm.
Above-mentioned graphite material refers to the graphite material prepared by chemical vapour deposition technique (CVD).
When graphite is prepared, if the base material for preparing is metal, the metallic substrates can be without removal;And if system Standby base material be insulating materials or the poor material of electric conductivity, then the substrate need removal.
2) minimum area and maximum area of graphite material needed for calculating, and according to this result of calculation, it is suitable in graphite Region cut out the graphite material of certain area;
Because longitudinal differential conductance of graphite has saturation value, so to calculate the minimum area S of required graphite materialG1.Profit Topography measurement is carried out to graphite surface with AFM (AFM), and according to the different purposes of pressure sensor, it is determined that required The range ability of the power of measurement, so as to calculate the area minimum area S of required graphite materialG1, computational methods are:
A. the shape appearance figure of graphite upper surface (i.e. the raised one side of surface folding), such as Fig. 2 are measured using AFM.According to the shape Looks figure, calculates the area of fold on graphite:In order to the convenience for calculating, the area of fold are quantified as a rectangle, its width is with pleat The halfwidth of wrinkle is calculated, and length is directly measured on shape appearance figure, and the gross area for being calculated fold is SW.And whole shape appearance figure is Square, its length of side can directly read from figure, be designated as L, then the area of whole scanning area graphite is L2.In order to be able to accurate Reflection fold accounts for the percentage of whole 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 is also unsuitable excessive (L≤30 μm).
B. in general, fold width exceeds well over the diameter of needle point, it is believed that the area of AFM probe needle point be needle point with The contact area of graphite fold, is designated as ST.For conduction mode AFM probe, needle point area is about 1200nm2
C. and according to pressure in Fig. 1 and the relation of differential conductance, when the pressure that needle point applies is more than 40nN, the electricity of fold Lead and be up to saturation value, at this moment fold will lose the measurement capability of power.Therefore, in order to realize the measurement of power exactly, needle point Pressure is no more than a fixed value FT, this value is typically 10-8The magnitude of N.
D. therefore, the maximum of the pressure for if desired measuring is FM, then the minimum area S of required graphiteG1Can 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, because:According to AFM in Fig. 2 to graphite surface The characterization result of pattern, it can be seen that the height of graphite surface each fold is different, and some crimp height is higher, Some crimp height is relatively low.When the pressure for applying is less, there is miniature deformation, relatively low pleat in fold only high There is no any deformation in wrinkle, the fold of this sub-fraction deformation is by so that pressure sensor realizes the accurate measurement of micro- power.Also It is to say, in order to realize the accurate measurement of micro- power, the total quantity of fold higher should not be excessive in the graphite for being used, because This, the maximum area S of the graphite for being usedG2Should meet:SG2=10 × SG1
When being characterized to graphite upper surface topography, the AFM pattern for using can be common contact pattern, Common tapping-mode, conduction mode, electrostatic force mode, magnetic mode, Kelvin Force pattern, peak value force mode or automatic mode Deng.
No matter the graphite material prepared using which kind of method, all there is impurity, broken hole and in uneven thickness etc. in its surface Problem.Accordingly, it would be desirable to the graphite regions for selecting clean, thickness homogeneous on graphite are used, to ensure made pressure sensing Power suffered by device is uniformly and stably dispersed in the regional of graphite material.
The small pieces graphite for being cut needs to be free of broken hole or broken hole area is smaller, but also the regular shape that need to be cut, with Just the gross area S of graphite can be calculatedG.The method of cutting can directly be cut using macro tools such as scissors, pocket knives, Can also use ultraviolet photolithographic, electron beam exposure, laser direct-write photoetching, nano-imprint lithography or focused-ion-beam lithography etc. micro- Machining tool is processed.
3) graphite material that will be cut out using conducting resinl sticks to the zone line on a piece of hard metal piece;
The conducting resinl for using should its have a stronger conductive capability, and can guarantee that 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 side in graphite material covers another hard metal piece, and the sheet metal is by gravity and the upper table of nickel foil Face contacts naturally, and the edge of two panels hard metal piece uses flexible insulating material adhesion, and whole pressure sensor is linked as into one Body, and realize encapsulation;
, it is necessary to coat a circle flexible insulating material, such as Fig. 3 along the edge of sheet metal before hard metal piece is covered. Then, another piece of hard metal piece is covered the upper surface of graphite.This block hard metal piece can be with due to Action of Gravity Field, both Fold on graphite is close to, again can be after flexible insulating material solidification, by the flexible insulating material and the metal of lower surface Piece forms adhesion, schematic diagram such as Fig. 4 of the pressure sensor.Two hard metal pieces of graphite surface covering, similar to two Electrode, when fixed voltage is applied on two sheet metals, just can measure the electric current on graphite direction with pressure Change, so as to calculate the change of corresponding differential conductance.
The hard metal piece for being used can be the metal simple-substance of all species or the alloy cpd of each metalloid.
Two hard metal pieces for covering can be the metal material, or different types of gold of same type Category material, but the area for being both needed to the graphite material than using facilitates greatly, so coats a circle flexible insulation material on sheet metal Material.
The flexible insulating material for being used should have stronger sticky, stronger flexible, preferable insulating properties and compared with Good sealing, can be dimethyl silicone polymer (PDMS), polymethyl methacrylate (PMMA), poly terephthalic acid second two Alcohol ester (PET), PEN (PEN), polytetrafluoroethylene (PTFE) (PTFE), polyimides (PI), makrolon (PC), Polyvinyl chloride (PVC), cellulose acetate (CA), polytrifluorochloroethylene (PCTFE) etc..Wherein, stronger viscosity can guarantee that two It is firm that sheet metal is adhered to;Stronger flexibility is to preferably realize the true measurement of pressure;Preferable insulating properties ensure Conductive path must be formed by graphite between two sheet metals;Preferable sealing can realize the good of the pressure sensor Good encapsulation.
5) pressure sensor is linked into respective measurement system, so as to realize that the pressure is passed in the measuring system The calibration of sensor.
In the pressure sensor, there is the authenticity of many factors meeting interference measurement results, such as graphite upper surface is hard The internal resistance that the gravity of matter sheet metal, the flexible material for using are introduced to 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 to the zero point of pressure.
In order to read the pressure value for measuring, in addition 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.So, a differential conductance value is often measured, just A specific pressure value can be corresponded to, so as to realize pressure sensing function.
Technical characterstic of the invention:There is the nano thickness graphite material of a large amount of folds in surface, perpendicular to its surface side Upward electric conductivity can be significantly increased with the increase of 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 scope of power that the pressure sensor can be measured is often larger, i.e. range It is larger.Again because the crimp height of graphite surface has certain difference, when pressure is smaller, a part only higher Fold stress, when the fold of stress is less, it is possible to achieve the detection to micro- power, thus the pressure sensor precision also very It is high.Further, since graphite material is nano thickness laminated structure, the pressure sensor also advantage with small volume.
Brief description of the drawings
Longitudinal differential conductance that Fig. 1 is measured at a fold using c-AFM on graphite is bent with the relation of fold stress Line;
The graphite surface shape appearance figure that Fig. 2 is measured using AFM;
The schematic diagram of pressure sensor when Fig. 3 covers hard metal piece not on graphite material;
The complete structure profile of Fig. 4 pressure sensors;
1-graphite material in figure;The fold on 2-graphite material surface;3-hard metal piece;4-conducting resinl;5-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 Help and further understand the present invention, but it will be appreciated by those skilled in the art that:The present invention and appended claims are not being departed from 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 defined by the scope that claims are defined.
Example 1:It is applied to the pressure sensor in precision balance.
1) appropriate area of the graphite prepared in CVD, uses common tapping-mode (the probe model OTESPA- of AFM R3 topography measurement) is carried out to graphite surface.
According to the shape appearance figure that measurement is obtained, the length of side L of shape appearance figure is 10 μm, and the fold in the shape appearance figure for calculating is total Area SWAbout 50 μm2.For general precision balance, it needs the maximum F of the pressure of measurementMGenerally 10N.By more than Data substitute into formulaIn, the minimum area S of required graphite can be calculatedG1It is 2.4 × 10-6m2
Precision balance needs to use precision pressure sensor higher, thus selected graphite material area not low It is as far as possible small under the requirement of minimum area, while to ensure to meet the demand of range, realize high-acruracy survey.
2) calculate for convenience, the suitable region on graphite, cut out the square graphite regions that the length of side is 2mm;
The use of a piece of length of side is the square graphite of 1cm, uses its surface topography of observation by light microscope, it is ensured that whole stone Graphite on ink sheet is clean, thickness is homogeneous and without broken hole.Then with the method for uv-exposure, paracentral area is met on graphite flake Domain exposes the square area that a length of side is 2mm, and the graphite of remainder is fallen using oxygen plasma etch.Exposure is finished Afterwards, using the acetone soak graphite flake, to remove the photoresist on surface.After removing photoresist, absolute alcohol and deionized water are used successively Clean, and dry up.
3) the circular hard copper sheet of a piece of a diameter of 3cm is taken, and area about 1cm is coated in region therebetween2Conductive silver Glue, the region of conductive silver glue covering should be approximately square, and the graphite material that then will be cut out at once sticks to the hard The region (one side that graphite material is posted on hard copper sheet is designated as front) of conductive silver glue is scribbled on copper sheet.Then by the hard copper Piece face-up stands 30 minutes, treats that conductive silver glue is spontaneously dried.
4) at the front proximal edge of hard copper sheet, upper circle PMMA glue is dripped, the track of drop glue is tried one's best circular hard The edge of copper sheet.The another side in the graphite material covers another hard copper sheet afterwards, and stands 2min, to ensure covering Hard copper sheet is close to graphite material.Pressure sensor will finally be carried out and toast 30min with 120 DEG C as on hot plate, make PMMA Solidification.
5) make pressure sensor one side fixed, another side is connected on an insulation bearing tray, and by two hard coppers Piece is connected with the both positive and negative polarity 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 counterweight such as 100g, 1000g, and being fitted using computer so that Complete the calibration to the pressure sensor.
Example 2:It is applied to the pressure sensor of ordinary electronic scale.
1) appropriate area of the graphite prepared in CVD, uses the common contact pattern (probe model SNL-10) of AFM Topography measurement is carried out to graphite surface.
According to the shape appearance figure that measurement is obtained, the length of side L of shape appearance figure is 20 μm, and the fold in the shape appearance figure for calculating is total Area SWAbout 80 μm2.For general ordinary electronic scale, it needs the maximum F of the pressure of measurementMGenerally 500N.Will be with Upper data substitute into formulaIn, the minimum area S of required graphite can be calculatedG1It is 4 × 10-4m2
2) calculate for convenience, the suitable region on graphite, cut out the square graphite regions that the length of side is 2cm;
Using light microscope, the graphite material is observed, and select clean, thickness homogeneous and without broken on its surface The region in hole, is cut out using pocket knife, finally obtains the square area that a length of side is 2cm.
3) the circular hard copper sheet of a piece of a diameter of 5cm is taken, and the patch lastblock length of side in region is about 2.5cm's therebetween Square conductive copper glue, the graphite material that then will be cut out sticks to the region that conductive copper glue is posted on the hard copper sheet surface (one side that graphite material is posted on hard copper sheet is designated as front).
4) at the front proximal edge of hard copper sheet, upper circle PDMS is dripped, the track of drop glue is tried one's best circular hard copper The edge of piece.The another side in the graphite material covers another hard copper sheet afterwards, and stands 2min, to ensure the hard of covering Matter copper sheet is close to graphite material.Pressure sensor will finally be carried out and toast 20min with 125 DEG C as on hot plate, and coagulate PDMS Gu.
5) make pressure sensor one side fixed, another side is connected on an insulation bearing tray, and by two hard coppers Piece is connected with the both positive and negative polarity 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 counterweight such as 5kg, and be fitted using computer, so as to realize to the pressure The calibration of sensor.
Example 3:It is applied to the pressure sensor of electronic product.
1) people more or less can apply certain when the Touch screen and touch pad of common electronic products is touched to it Pressure, the scope of general pressure is 10-2Change between~1N.And general electronic products use common Touch screen and common Touch pad, although they can respond touch operation, the size of None- identified pressure.Cause common Touch screen and common The small-sized electronic products such as touch pad realize the response to pressure, it is necessary to coordinate relatively thin, more accurate pressure sensor.So choosing The graphite material containing more fold of CVD preparation is taken, and it is right with the common contact pattern (probe model SNL-10) of AFM Graphite surface carries out topography measurement.
According to the shape appearance figure that measurement is obtained, the length of side L of shape appearance figure is 20 μm, and the fold in the shape appearance figure for calculating is total Area SWAbout 80 μm2.The pressure of common people's Touch screen is general 10-2In the range of~1N.Data above is substituted into formulaIn, the minimum area S of required graphite can be calculatedG1It is 6 × 10-7m2
2) calculate for convenience, the suitable region on graphite, cut out the square graphite regions that the length of side is 1mm;
The use of a piece of length of side is the square graphite flake of 1cm, uses their surface topography of observation by light microscope, it is ensured that Graphite on the graphite flake is clean, thickness is homogeneous and without broken hole.Then with the method for uv-exposure, close to center on graphite flake Regional exposure go out the square area that a length of side is 1mm, the graphite of remainder fallen using oxygen plasma etch.Exposure After finishing, 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) take a piece of length of side be 2cm square thin hard copper sheet, and the thin hard copper sheet zone line apply above Product is about 1cm2Conductive silver glue, the region of conductive silver glue covering should be approximately square, the graphite that then will be cut out at once Material sticks to and the region of conductive silver glue is scribbled on the thin hard copper sheet (one side that graphite material is posted on hard copper sheet is designated as just Face).Then the hard copper sheet is face-up stood 30 minutes, treats that conductive silver glue is spontaneously dried.
4) at the front proximal edge of thin hard copper sheet, the appropriate PDMS of a upper circle is dripped, the track for dripping glue tries one's best just The edge of square thin hard copper sheet.The another side in graphite material covers another hard scale copper afterwards, and stands 2min, with Ensure 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 Baking 20min, solidifies PDMS.
5) pressure sensor is corrected:Timing, two hard scale coppers of pressure sensor respectively with one The both positive and negative polarity connection of precision ammeter.Then, measure respectively and calculate it is unloaded and apply on hard scale copper 0.01N, The corresponding differential conductance value of the power such as 0.1N, 1N, and be fitted using computer, so as to complete the school to the pressure sensor It is accurate.
Although the present invention is disclosed as above with preferred embodiment, but is not limited to the present invention.It is any to be familiar with ability The technical staff in domain, in the case where technical solution of the present invention ambit is not departed from, all using in the methods and techniques of the disclosure above Appearance makes many possible variations and modification, or the Equivalent embodiments for being revised as equivalent variations to technical solution of the present invention.Therefore, Every content without departing from technical solution of the present invention, according to technical spirit of the invention to made for any of the above embodiments any simple Modification, equivalent variations and modification, still fall within the range of technical solution of the present invention protection.

Claims (10)

1. a kind of pressure sensor, it is characterised in that there is the graphite material of fold including-surface, the graphite material is nanometer Thickness laminated structure;The graphite material sticks to the zone line on a piece of hard metal piece;Another hard metal piece covers Cover on graphite material, above-mentioned two panels hard metal piece edge is using flexible insulating material adhesion and encapsulates.
2. a kind of preparation method of pressure sensor, comprises the following steps:
1) graphite material that surface has fold is prepared, the graphite material is nano thickness laminated structure;
2) topography measurement is carried out to graphite material surface using AFM, selection is clean, the homogeneous region of thickness, according to pressure The range ability of measurement power cuts graphite material needed for force snesor;
3) above-mentioned graphite material is sticked to the zone line on a piece of hard metal 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 flexibility Insulating materials adhesion is simultaneously encapsulated, and forms pressure sensor as claimed 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 accurate.
3. preparation method as claimed in claim 1, it is characterised in that step 1) described in the average thickness of graphite material be 10 ~500nm.
4. preparation method as claimed in claim 1, it is characterised in that step 1) described in graphite material be to use chemical gaseous phase Graphite material prepared by sedimentation CVD.
5. preparation method as claimed in claim 1, it is characterised in that step 2) described in AFM measurement mould Formula is common contact pattern, common tapping-mode, conduction mode, electrostatic force mode, magnetic mode, Kelvin Force pattern, peak value Force mode or automatic mode.
6. preparation method as claimed in claim 1, it is characterised in that step 3) described in conducting resinl be 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 there is excellent conductive The glue of ability.
7. preparation method as claimed in claim 1, it is characterised in that step 3) described in cutting method be scissors, it is small The direct cutting that the macro tools such as knife are carried out, or ultraviolet photolithographic, electron beam exposure, laser direct-write photoetching, nano-imprint lithography or The processing that the micro Process such as focused-ion-beam lithography instrument is carried out.
8. preparation method as claimed in claim 1, it is characterised in that step 3) and step 4) described in hard metal piece be Refer to the metal simple-substance of all species or the alloy cpd of each metalloid.
9. preparation method as claimed in claim 1, it is characterised in that step 4) described in flexible insulating material refer to poly- two Methylsiloxane, polymethyl methacrylate, polyethylene terephthalate, PEN, polytetrafluoroethyl-ne Alkene, polyimides, makrolon, polyvinyl chloride, cellulose acetate, polytrifluorochloroethylene.
10. preparation method as claimed in claim 1, it is characterised in that step 5) described in calibration refer to corresponding measurement System carries out zero correction and the correction of the corresponding pressure value of corresponding scale division value.
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CN112932188A (en) * 2021-01-28 2021-06-11 江苏经贸职业技术学院 Plate component of retail container and intelligent retail container

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