CN105300574A - Graphene pressure sensor, manufacturing method thereof and purpose thereof - Google Patents
Graphene pressure sensor, manufacturing method thereof and purpose thereof Download PDFInfo
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- CN105300574A CN105300574A CN201510780886.0A CN201510780886A CN105300574A CN 105300574 A CN105300574 A CN 105300574A CN 201510780886 A CN201510780886 A CN 201510780886A CN 105300574 A CN105300574 A CN 105300574A
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- 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
- G01L1/18—Measuring 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 provides a graphene pressure sensor and a manufacturing method thereof. The graphene pressure sensor is characterized in that the graphene pressure sensor is at least composed of an elastic substrate layer, a graphene pressure sensing layer and a packaging layer, wherein the elastic substrate layer comprises a sensing area, an overlapping area and an electrode area; the graphene pressure sensing layer is attached to the sensing area, and the graphene pressure sensing layer is in direct contact with the electrode area so as to form the overlapping area; the packaging layer covers the graphene pressure sensing layer and the overlapping layer between the graphene pressure sensing layer and the electrode area. The graphene pressure sensor is high in sensitivity, good in stability and long in expected service lifetime, in addition, the manufacturing cost is low, the process is simple, and the process is controllable.
Description
Technical field
The present invention relates to Graphene pressure transducer and its production and use.
Background technology
Present electric capacity touch screen is only relatively elementary input, and they just follow the trail of the track moving formation at the finger of screen surface or the position of stylus.The defect using touch Panel is that they can not provide the information of pressure or size of exerting pressure usually, and the size of pressure also can be used as another dimension of input, and it can provide instruction or control signal for the electronic equipment of associated.
The higher diaphragm pressure sensor of current sensitivity adopts ZnO nanowire array or Kynoar (PVDF) as induction sensitive element mostly, but sensitivity is still not high enough, accurately induction is difficult to for the pressure deformation strained lower than 0.4%, also just larger to the seizure difficulty of signal when microcircuit design like this.
For extremely faint strain (<0.4%), ZnO or PVDF piezoelectric pressure indicator induction skip signal is not just clearly, seizure to setting pressure signal when being so just unfavorable for microcircuit design, is also just difficult to carry out digital algorithm signal transacting;
In addition, ZnO pressure sensitivity tactility apparatus is more responsive to acid, aqueous slkali, easily chemical reaction occurs, and particularly for electronic product that is frequent and human contact, can have a strong impact on the stability of sensor.
Patent CN104359597A discloses a kind of pressure transducer, the pressure transducer of the miniature change of this induction is with two sheets of flexible substrate and the carbon nano-tube or the graphene film that cover inside surface respectively, electrode lays respectively at two ends inside two sheets of flexible substrate, two layers of substrate staggers assembling, when being squeezed, the external forces such as stretching time, the contact area of upper and lower two layer graphenes (or carbon nano-tube) layer will change, thus cause the contact resistance of two interlayers to change.Although this sensor also has very high sensitivity, but this sensor is because levels Graphene or carbon nano-tube can not encapsulate, easily damage in using, and this sensor is also relevant with the factor such as difference in height and profile pattern in levels gap, and the stability of pressure sensitive signal is very poor.
Therefore, still need to develop highly sensitive, good stability, long service life pressure transducer.
Summary of the invention
For solving the problem, the invention provides a kind of Graphene pressure transducer, it is characterized in that, it is at least made up of elastic substrate layer, Graphene pressure sensitive layer and encapsulated layer;
Wherein said elastic substrate layer comprises induction zone, overlap and electrode district;
Described Graphene pressure sensitive layer is attached on induction zone, and Graphene pressure sensitive layer directly contacts with electrode district and forms overlap; Described encapsulated layer covers the overlap of Graphene pressure sensitive layer and Graphene pressure sensitive layer and electrode district.
In the present invention, described electrode district is used for flexible print circuit (FPC) structural region that polymeric membrane and metal electrode form; Induction zone is used for the high-molecular organic material composite structure region of placing graphite alkene pressure sensitive layer; Overlap is the metal electrode region will contacted with Graphene pressure sensitive layer.
Wherein said high-molecular organic material comprises but is not limited to bonding agent, rubber, plastics or resin.
In addition, the invention provides a kind of also method preparing above-mentioned Graphene pressure transducer, it is characterized in that, said method comprising the steps of:
(1) on supporting layer, make elastic substrate layer, make surface, electrode district and surface, induction zone at grade;
(2) Graphene pressure sensitive layer is prepared;
(3) Graphene pressure sensitive layer is transferred to induction zone, and guarantees that Graphene pressure sensitive layer and electrode district form effective overlap joint;
(4) etching induction pattern on Graphene pressure sensitive layer;
(5) to Graphene pressure sensitive layer and overlap coating high-molecular organic material, encapsulated layer is formed;
(6) according to required physical dimension cutting product sensor.
The present invention also provides above-mentioned Graphene pressure transducer for the purposes of intelligent terminal.
Graphene Sensitivity in Pressure Sensors of the present invention is high, good stability, expected service life are long, and its cost of manufacture is low, technique is simple and easy, process control.
Accompanying drawing explanation
Fig. 1 is a kind of front elevation of Graphene pressure transducer.
Fig. 2 is a kind of vertical view of Graphene pressure transducer.
The pressure sensitivity signal of sensor when Fig. 3 is finger flicking.
Fig. 4 is the heavy sensor pressure sensitivity signal on time of finger.
Embodiment
In the present invention, about the location expression of each several part in Graphene pressure transducer, be based on attached Fig. 1 and 2, obviously, along with the evolution of accompanying drawing 1-2 equipment, wherein the position of each parts also changes; Therefore, this instructions does not form any restriction to invention in conjunction with the explanation of particular location.
The invention provides a kind of Graphene pressure transducer, it is characterized in that, it is at least made up of elastic substrate layer, Graphene pressure sensitive layer, encapsulated layer;
Wherein said elastic substrate layer comprises induction zone, overlap, electrode district;
Described Graphene pressure sensitive layer is attached on induction zone, and Graphene pressure sensitive layer directly contacts with electrode district and forms overlap; Described encapsulated layer covers the overlap of Graphene pressure sensitive layer and Graphene pressure sensitive layer and electrode district.
In the present invention, described elastic substrate layer comprises induction zone, overlap, electrode district; Wherein electrode district is used for the flexible printed circuit structure region that polymeric membrane and metal electrode form; Induction zone is used for the high-molecular organic material composite structure region of placing graphite alkene pressure sensitive layer; Overlap is the metal electrode region will contacted with Graphene pressure sensitive layer.
Wherein said high-molecular organic material comprises but is not limited to bonding agent, rubber, plastics or resin.
In the present invention, described electrode is positioned at the homonymy of Graphene pressure transducer, is not only easy to binding, and makes pressure sensitivity region larger, can also be conducive to the Graphene of the interface of guard electrode and elastic substrate layer like this.Encapsulated layer covers the overlap of Graphene pressure sensitive layer and Graphene pressure sensitive layer and electrode district, contributes to the stable of final products and protection like this, guarantees the Long-Time Service of product.
In addition, the invention provides a kind of method preparing above-mentioned Graphene pressure transducer, it is characterized in that, said method comprising the steps of:
(1) on supporting layer, make elastic substrate layer, make surface, electrode district and surface, induction zone at grade;
(2) Graphene pressure sensitive layer is prepared;
(3) Graphene pressure sensitive layer is transferred to induction zone, and guarantees that Graphene pressure sensitive layer and electrode district form effective overlap joint;
(4) etching induction pattern on Graphene pressure sensitive layer;
(5) to Graphene pressure sensitive layer and overlap coating high-molecular organic material, encapsulated layer is formed;
(6) according to required physical dimension cutting product sensor.
In step (1), described supporting layer can be double faced adhesive tape, one side release liners, one side glue, polyester film, PET (polyethylene terephthalate), PI (polyimide), PE (tygon), PP (polypropylene), PVC (Polyvinylchloride), PBT (polybutylene terephthalate), PMMA (polymethylmethacrylate), metal, pottery and flexible glass, wherein, supporting layer makes the making of the elastic substrate layer connected with electrode side be more prone to, simultaneously can avoid breaking of electrode and elastic substrate bed interface place's Graphene in manufacturing process, play a protective role.
In step (1), for increasing the interfacial contact area of electrode district and induction zone, the electrode place adjacent with induction zone, its xsect can be serrate or waveform etc.
In step (1), described induction zone can be the various eiastomeric silicone glue of acid and alkali-resistance etch, stable chemical nature compatible good with human-body biological, it can be selected from PDMS (dimethyl silicone polymer), silica gel E620 (dimethyl diphenyl polysiloxane), OCA glue (transparent optical cement), its thickness is 10-250 μm, be preferably 50-200 μm, be more preferably 100-175 μm.
In a preferred embodiment, in step (1), be coated on supporting layer after elastic silica gel vacuum stripping is steeped, make its surface and electrode surface at grade, degassed under vacuum bubble, is then heating and curing again, form elastic substrate layer, wherein said heating is carried out in an oven, and heating-up temperature is 30-150 DEG C, and set time is 10-180min.
In another preferred embodiment of the present, in step (1), the back side, electrode district and induction zone and supporting layer are pasted, use volume to volume roll extrusion that three is closely pasted, and make induction zone and surface, electrode district at grade.
In another preferred embodiment of the present, in step (1), also Copper Foil can be pressurizeed with induction zone together with supporting layer, be corroded by the film, obtain the electrode of required pattern.
In step (2), described Graphene pressure sensitive layer is prepared by methods known in the art, such as chemical vapour deposition technique (CVD), or also by graphene powder is prepared graphene film through coating, roll extrusion, suction filtration, spraying, or use graphene oxide powder to form graphene oxide film through coating, roll extrusion, suction filtration, spraying, form graphene film by reducing process again, form graphene film with patterning process.
When using process for preparing graphenes by chemical vapour deposition pressure sensitive layer, the substrate of growing graphene used includes but not limited to the sheet material of copper, iron, nickel, cupronickel, monox, silit, platinum, net material and three-dimensional foam structure material.
In a preferred embodiment, in step (2), described Graphene pressure sensitive layer uses CVD preparation, and the thickness of wherein said graphene net is 10-500nm, mesh is 10 × 10-500 × 500 μm, and single Graphene live width is 5-250 μm.
In step (2), the sheet resistance of prepared Graphene pressure sensitive layer is 0.2-200K Ω/.
In step (4), etching adopts laser etching machine to carry out, and described laser etching machine is the laser etching machine that this area routine uses, and it can be buied.
In step (4), for the Graphene and surrounding Graphene pressure sensitive layer guaranteeing induction pattern disconnects, and obtain relatively larger pressure sensitive region, described induction pattern can be the patterns such as concentric many prescriptions shape, circle, ellipse.
In step (4), the distance of described line influence pattern and right side edge is 0.01-10mm, is preferably 0.1-6mm, and the width of induction pattern outermost pattern is 0.01-1mm, is preferably 0.2-5mm.
In a preferred embodiment, in step (5), for preventing the electrode district away from overlap from not applying high-molecular organic material, masking tape can be used to protect electrode, and described adhesive tape is pressure sensitive adhesive tape.
In step (5), for making the organic polymer of coating solidify, can heat in an oven, oven temperature is 30-150 DEG C, and set time is 5-180min.
In step (5); described encapsulated layer can be various organic silica gel; it can be selected from PDMS, silica gel E620, C6-515 liquid silica gel; described encapsulated layer thickness can be 10 ~ 500 μm; be preferably 50-300 μm; be more preferably 100-200 μm, avoid to protect Graphene pressure sensitive layer scratching.
In a preferred embodiment, in step (5), stress damage is subject to for preventing overlap, encapsulated layer upper surface adhesion interface reinforcing band above overlap, described interface reinforcing band is optional from pressure sensitive adhesive, UV-curing glue, hot-setting adhesive, instant drying adhesive, structure glue, fluid sealant.
In a preferred embodiment, the electrode of described electrode district is flexible print circuit (FPC) electrode, it is made up of Copper Foil and PI film, wherein the thickness of PI film is 10-500 μm, PI film and Copper Foil are processed according to heat pressing process hot pressing well known in the art and form electrode, described copper foil surface can evaporation thickness be the anti oxidation layer of 10-500nm, and described anti oxidation layer can be gold, nickel or nickel-chrome.
In the present invention, on Copper Foil, gold evaporation, nickel or nickel-chrome can prevent the corrosion of the iron chloride remained in graphene mesh or the corrosion of other bronsted lowry acids and bases bronsted lowry, and then can guarantee the stability of sensor.
In another embodiment, the electrode of described electrode district is FPC electrode, and it is PET (polyethylene terephthalate) copper plating film, and can the anti oxidation layer of the golden film of evaporation thickness 10-500nm, nickel film or nickel-chrome on copper.
In the present invention, those skilled in the art can change the static resistance because usually changing described Graphene pressure transducer such as structure and thickness of elastic substrate layer in graphite pressure transducer and encapsulated layer material used and Graphene pressure sensitive layer, described static resistance is 0.2-200K Ω, preferred 1.0-100K Ω, more preferably 2-50K Ω, can the scope of induction pressure be 0.1g-100kg, be preferably 1.0g-50kg, more preferably 20g-10kg.
In the present invention, the present invention adopts on-deformable Copper Foil to make follow-up direct test, welding or binding can not damage Graphene pressure sensitivity region easily, is conducive to the stability of sensor.
The miniaturization structure of Graphene pressure transducer of the present invention can be assemblied in frame place or the LCD back side of smart mobile phone, and the pressure sensitivity that can also obtain another dimension is experienced.
The present invention also provides above-mentioned pressure transducer for the purposes of intelligent terminal, and Graphene pressure transducer of the present invention can be used for smart mobile phone, wearable electronic etc.
Below in conjunction with accompanying drawing, the invention will be further described, but be not intended to limit the present invention.
Embodiment
Example one
The FPC electrode back side (i.e. PI film side) be made up of PI film 3 (thickness is 125 μm) and the Copper Foil 4 (thickness is 30 μm) of gold evaporation (thickness is 200nm) is closely bonded with supporting layer double faced adhesive tape and release liners 1; The A of organic silica gel E620, B component mixed according to 1:1 and is coated in supporting layer double faced adhesive tape and release liners 1 after de-bubble under vacuo, then putting into 80 DEG C, baking oven, 40min is heating and curing, as induction zone 2.
Adopt atmospheric pressure cvd method growing graphene, its substrate is 200 order copper mesh, and brass wire diameter is 45 μm, and mesh is 75 × 75 μm, and prepared Graphene thickness is 80 ~ 100nm, and the single width of graphene net is 70 μm, and aperture is 66.5 × 66.5 μm.
The copper mesh of Graphene is had to lie against FeCl growth
3in solution by copper mesh corrosion completely, the FeCl repeatedly will remained in graphene mesh is cleaned with pure water
3solution cleans up, then the Graphene of above-mentioned preparation is transferred on substrate surface, and make graphene mesh and electrode form effective overlap joint, the substrate of wherein said transfer Graphene comprises electrode district, induction zone, supporting layer, and put and naturally dry to air, this example Graphene pressure sensitive layer sheet resistance is 50K Ω/;
Pressing design laser etching machine etches concentric collar rectangle induction pattern 7, and to increase induction region as far as possible, induction pattern 7 is about 1mm apart from right side edge, and induction pattern 7 outermost square pattern width is about 0.3mm.
Paste on Copper Foil 4 from left end 1/4-3/4 length areas pressure sensitive adhesive tape, then mixing adds organic silica gel E620, vertically static again after level, make graphenic surface uniform fold one deck organic silica gel E620, its thickness is about 0.15mm, then put in baking oven 80 DEG C, 40min is heating and curing, as encapsulated layer 6, finally the pressure sensitive adhesive tape be attached on electrode is torn.
Encapsulated layer upper surface sticking two-faced adhesive tape 8 above Copper Foil 4 with induction zone 2 contact interface, then according to design sensor shape size, by the outer shape of cut sensor, make it be separated with substrate, the static resistance of gained Graphene pressure transducer is 1.0k Ω.
Embodiment 2
The FPC electrode back side (i.e. PI film side) form the Copper Foil 4 (thickness is 25 μm) by PI film 3 (thickness is 80 μm) and evaporation nickel-chrome (thickness is 150nm) and supporting layer one side PET adhesive tape 1 are closely pasted, make two-layer between do not produce gap and bubble; The host of PDMS and hardening agent are mixed vacuum according to 10:1 go down after bubble removing to be coated on supporting layer one side glue polyester tape 1, leave standstill 60min nature levelling, make its surface with Copper Foil 4 at same plane, then again bubble removing is vacuumized, then to put in baking oven 60 DEG C, 70min is heating and curing, as induction zone 2, finally silica gel residual on Copper Foil 4 is removed.
Adopt atmospheric pressure cvd method, graphene growth substrate is 100 order copper mesh, brass wire diameter 100 μm, mesh 150 × 150 μm, prepared Graphene thickness 150 ~ 180nm, and the single width of graphene net is 120 μm, 130 × 130 μm, aperture.
Copper mesh after growing graphene is lain against FeCl
3in solution by copper wire corrosion completely, the FeCl will remained in graphene mesh is repeatedly cleaned with high purity water
3solution cleans up, then cleaning Graphene is repeatedly transferred on substrate surface, the substrate of described transfer graphene mesh comprises electrode district, induction zone, supporting layer, then put and naturally dry to air, Van der Waals force is relied on to make Graphene be adsorbed on surface, induction zone 2, and making Graphene and electrode form effective overlap joint, the graphene net of substrate surface is as Graphene pressure sensitive layer 5, and gained Graphene pressure sensitive layer sheet resistance is 100 Ω/;
Pressing design laser etching machine etches concentric collar rectangle induction pattern 7, and to increase induction region as far as possible, induction pattern 7, apart from right side edge 0.6mm, responds to pattern 7 outermost square pattern width 0.2mm.
Paste on Copper Foil 4 from left end 1/4-3/4 length areas pressure sensitive adhesive tape, then drip and mix ground PDMS, horizontal rest 60min, nature levelling, make graphenic surface uniform fold one deck PDMS, thickness is about 0.2mm, then to put in baking oven 60 DEG C, 120min is heating and curing, as encapsulated layer 6, finally the pressure sensitive adhesive tape be attached on electrode is slowly torn.
Encapsulated layer upper surface above Copper Foil 4 with induction zone 2 contact interface is coated with the polyimide resin 8 of 0.2mm thickness, then according to design sensor shape size, by the outer shape of cut sensor, make it be separated with substrate, the static resistance of gained Graphene pressure transducer is 50K Ω.
Example three
To be the OCA glue of 175 μm and thickness be that the PET1 of 125 μm pastes for the back side (i.e. PI film side) of the FPC electrode formed by the Copper Foil 4 (thickness is 20 μm) by PI film 3 (thickness is 50 μm) and evaporation nickel (thickness is 250nm) and thickness, release film is covered in front, with volume to volume roll extrusion, three is closely pasted again, gap and bubble is not produced between each layer, make OCA glue surface with copper foil electrode 4 at same plane, OCA glue is as induction zone 2.
Adopt atmospheric pressure cvd method, graphene growth substrate is 80 order copper mesh, brass wire diameter 50 μm, mesh 200 × 200 μm, prepared Graphene thickness 55nm, and the single width of graphene net is 74 μm, 184 × 184 μm, aperture.
Copper mesh after growing graphene is lain against FeCl
3by complete for copper wire corrosion in solution, more repeatedly clean the FeCl will remained in graphene mesh with high purity water
3solution cleans up, then cleaning Graphene is repeatedly transferred to substrate surface, Graphene and electrode is made to form effective overlap joint, the substrate of described transfer Graphene comprises electrode district, induction zone, supporting layer, 60 DEG C, after 60min heat drying, rely on Van der Waals force to make it be adsorbed on surface, induction zone 2, the graphene net of substrate surface is as Graphene pressure sensitive layer 5, and gained Graphene pressure transducer sheet resistance is 600 Ω/;
Pressing design laser etching machine etches concentric collar rectangle induction pattern 7, and increasing induction region, induction pattern 7, apart from right side edge 0.8mm, responds to pattern 7 outermost square pattern width 0.35mm.
By on Copper Foil 4 from the light applying adhesive tape of left end 1/4-3/4 length areas, then drip mix by C6-515 liquid silica gel (dimethyl diphenyl polysiloxane), horizontal rest 40min, vertically hang 15min again, make graphenic surface uniform fold one deck silica gel C6-515 liquid silica gel, thickness is about 0.1mm, then to put in baking oven 70 DEG C, 40min is heating and curing, as encapsulated layer 6, finally the pressure sensitive adhesive tape be attached on electrode is slowly torn.
Encapsulated layer upper surface above Copper Foil 4 with induction zone 2 contact interface is coated with the phenolics 8 of 0.2mm thickness, then according to the sensor shape size of design, by the outer shape of cut sensor, make it be separated with substrate, the static resistance of gained Graphene pressure transducer is 0.5K Ω.
The Graphene pressure transducer prepared by embodiment 1 is simulated the complete machine assembling test with mobile phone, is positioned on substrate, attach the elastic foam identical with sensor thickness around sensor, add one deck hard cover plate above.External Force Acting is when cover plate, and foam compresses, and sensor also strain signal occurs thereupon, and test result as shown in Figure 3 and Figure 4.
Claims (10)
1. a Graphene pressure transducer, it is at least made up of elastic substrate layer, Graphene pressure sensitive layer, encapsulated layer;
Wherein said elastic substrate layer comprises induction zone, overlap, electrode district;
Described Graphene pressure sensitive layer is attached on induction zone, and Graphene pressure sensitive layer directly contacts with electrode district and forms overlap; Described encapsulated layer covers the overlap of Graphene pressure sensitive layer and Graphene pressure sensitive layer and electrode district.
2. Graphene pressure transducer according to claim 1, wherein said Graphene pressure sensitive layer is graphene net.
3. Graphene pressure transducer according to claim 1 and 2, the sheet resistance 0.1-10 of wherein said Graphene pressure sensitive layer
6Ω/, the static resistance of wherein said Graphene pressure transducer is 0.2-200K Ω, can the scope of induction pressure is 0.1g-100kg.
4. Graphene pressure transducer according to claim 1, wherein, described electrode district is the flexible print circuit be made up of polymeric membrane and metal electrode, and described polymeric membrane is PI, PET, PE, PMMA film; Described induction zone is high-molecular organic material, and described macromolecular material is organic silica gel, rubber or plastics.
5. Graphene pressure transducer according to claim 1, wherein, described encapsulated layer is organic silicone oil, silicon rubber, silicones, and described encapsulated layer prints technique formation by some glue, spraying, coating, serigraphy and 3D.
6. prepare a method for Graphene pressure transducer described in claim 1, it comprises the following steps:
(1) on supporting layer, make elastic substrate layer, make surface, electrode district and surface, induction zone at grade;
(2) Graphene pressure sensitive layer is prepared;
(3) Graphene pressure sensitive layer is transferred to induction zone, and guarantees that Graphene pressure sensitive layer and electrode district form effective overlap joint;
(4) etching induction pattern on Graphene pressure sensitive layer;
(5) to Graphene pressure sensitive layer and overlap coating high-molecular organic material, encapsulated layer is formed;
(6) according to required physical dimension cutting product sensor.
7. method according to claim 6, wherein, in step (1), described supporting layer is double faced adhesive tape, one side release liners, one side glue, polyester film, PET, PI, PE, PP, PVC, PBT, PMMA, metal, pottery and flexible glass.
8. method according to claim 6, wherein, in step (2), described Graphene pressure sensitive layer uses graphene powder to form graphene film through coating, roll extrusion, suction filtration, spraying, or use graphene oxide powder to form graphene oxide film through coating, roll extrusion, suction filtration, spraying, form graphene film through reducing process again, then form the preparation of Graphene pressure sensitive layer with patterning process or use chemical vapour deposition technique preparation.
9. method according to claim 6, wherein, in step (2), described Graphene pressure sensitive layer uses chemical deposition preparation, and wherein substrate used is copper, iron, nickel, cupronickel, monox, silit, the sheet material of platinum, net material and three-dimensional foam structure material.
10. the Graphene pressure transducer described in claim 1-5 is used for the purposes of smart mobile phone, wearable electronic.
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| PCT/CN2016/076062 WO2017080128A1 (en) | 2015-11-13 | 2016-03-10 | Graphene pressure sensor and manufacturing method and use thereof |
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| CN105300574B (en) | 2018-04-17 |
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