CN102506693A - Graphene-based strain measuring and motion sensing device and manufacturing method thereof - Google Patents
Graphene-based strain measuring and motion sensing device and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a graphene-based strain measuring or motion sensing device. The device is formed by the following steps: a layer or a plurality of layers of graphene film layers are combined on a flexibly insulating substrate; two ends of the graphene film layer are led out through electrodes and connected with ohmmeters, wherein the device is closely combined on the surface of an object to be detected, or a plurality of the devices are closely combined on the surface of the object to be detected, so that the strain variation measurement or motion monitoring can be realized. The device disclosed by the invention has the advantages of simple manufacturing method and capabilities of being suitable for large-scale production such as surface mounting and the like, and being applied to various types of environments and deformed surfaces; especially, the influence on the object to be detected is small, so that contactless measurement can be realized, and the device is suitable for monitoring biological motion. The invention further discloses a manufacturing method and a measuring method for the device.
Description
Technical field
The present invention relates to a kind of strain measurement and motion sensor means based on Graphene and preparation method thereof.
Background technology
Graphene has high physical strength, the electronic transport performance of excellence and good chemically-resistant environment capacity, and as the thinnest material, it can adhere at various surface-stables, and changes shape along with changes in surface.Particularly, existing discovering when Graphene is stretched or during compression, tangible change can take place its resistance, and changes within the specific limits and is good linear relationship.
Existing strain sensing and measuring method have following several types:
The metal species foil gauge serves as to measure sensing unit with metal forming or metal wire usually, and the metal forming through special shape design or processing is the strain sensing unit, through the resistance change measurement strain, like Chinese patent 200710096310.8,200510078142.0 etc.
The conducting polymer strain measurement, the substrate or the fabric that have electroconductive polymer coating or coating can be responded to strain, but bad mechanical property, fatiguability is aging.Use carbon nano tube compound material can improve its performance to a certain extent, like Chinese patent 200910252377.5.
The optical strain sensor is measured relative motion and strain with optical instruments such as optical fiber, gratings, like one Chinese patent application 200880012635.6.
Semiconductor strain sensor like strained silicon, germanium etc., utilizes the change of the strained back of semiconductor performance, like Chinese patent 200710109001.X.
Compare with above-mentioned strain measurement method; Based on the strain measurement and the motion sensor means of Graphene, simple in structure, be quick on the draw, more tolerate fatigue and environmental change, can be extended to the different scale from the micron to rice; And can use on various surfaces, have wide application space.
Summary of the invention
The present invention utilizes the linear relationship of Graphene resistance and strain, and combine the Graphene softness simultaneously, can well contact with various surfaces, thus the synchronous perception adaptability to changes of ability, to obtain novel strain measurement and motion measuring method.
The purpose of this invention is to provide a kind of strain measurement and motion-sensing method based on Graphene, with and related device and method for making.
The present invention is based on following two performances or the principle of Graphene: (1). Graphene can be good is attached to various measured surfaces; When measured surface generation deformation; Graphene is owing to have only atom level thickness, thus can be synchronous fully follow measured surface deformation and influence measured surface deformation hardly.(2) Graphene is stretched or during compressive strain, resistance has obvious variation, and within the specific limits, resistance variations and strain linear (as shown in Figure 3).
In conjunction with the These characteristics of Graphene, technical scheme of the present invention is following:
A kind of based on the strain measurement of Graphene or the device of motion-sensing; It is characterized in that: it is in the substrate of flexible insulation, to be combined with one or more layers graphene film layer; The two ends of graphene film layer are drawn with electrode and are connected ohmmeter; This device is combined closely in testee surface, or a plurality of these devices are combined closely to measure this testee surface strain variations in the testee surface or carry out motion-sensing.
Above-mentioned device; Described flexible insulation substrate can be the macromolecule flexible polymeric materials, like tygon, PVC, teflon, polypropylene, polyethylene terephthalate (PET), polymethylmethacrylate (PMMA), dimethyl silicone polymer (PDMS) etc.; Also can be composite and flexible material, inorganic fexible film or the gel rubber material of the surface of stability is arranged.
Above-mentioned device, described electrode are metals such as gold, silver, copper, chromium, titanium, aluminium, platinum, or other is like the film of indium tin oxide high conductivity such as (ITO).
Above-mentioned device, graphene layer can be the band shape or the line image of aspect ratio.
Above-mentioned device can be combined closely many Graphene bands on same flexible substrates with different angles through repeatedly shifting, and also can Graphene lamella bigger on the flexible substrates be etched into many Graphene bands through the plane processing technology; Every paired extraction electrode in Graphene band two ends makes a device can measure the strain or the motion of different directions simultaneously;
Above-mentioned device, a plurality of these devices can be connected in series, and with the resistance variations signal that obtains to strengthen, improve and measure sensitivity.
Above-mentioned device, a plurality of independently these flexible apparatus can be used stacked system, put, combine closely in same measured surface with the different angles shop, to obtain the strain or the movable information of different directions.
A kind of method for preparing above-mentioned strain measurement or motion sensor means, it may further comprise the steps:
1. the substrate (like copper, nickel etc.) of preparing to be used to grow Graphene is prefabricated into required form, cleans, then oven dry;
2. on growth substrate, deposit Graphene; Representative condition is: with 25 micron copper foils is substrate, keeps 1000 ℃ of growth temperatures, feeds methane and hydrogen; Gas flow is methane 25sccm; Hydrogen 10sccm grew after 15 minutes, closed methane; Under the protection of 10sccm hydrogen gas stream, be cooled fast to room temperature, on copper, obtain the graphene film that the number of plies is the 1-2 layer;
3. graphene film is transferred on the required flexible substrates, can be passed through repeatedly transfer method and in same substrate, lay many Graphenes.Typical transfer method is that elder generation is coated with PMMA glue at the copper foil surface of the Graphene of growing, and the graphene layer on copper surface and PMMA layer are adhered to; Place the 0.1M ferric chloride solution to soak 24 hours Copper Foil then, erode Copper Foil, the remaining Graphene hyaline membrane that is combined with PMMA; Afterwards can be directly on this film extraction electrode use, also (like PET, PDMS etc.) back re-uses with acetone flush away PMMA in other substrates so that this film is attached at again.
4. prepare electrode at Graphene band two ends, and draw circuit.
Above-mentioned preparation method, the growth substrate described in the step 1 can be processed required form in advance, also can behind the growth Graphene, be reprocessed into required form.
Above-mentioned preparation method, the Graphene growing method described in the step 2 can be chemical vapor deposition (CVD), plasma reinforced chemical vapour deposition (PECVD), metal surface epitaxial growth etc.
The method that above-mentioned preparation method, step 4 prepare electrode can be directly to be coated with conducting resinl, also can use the standard silk-screen printing technique, or ion sputtering, electron beam evaporation, hot vapor deposition or magnetron sputtering equal vacuum coating process deposit all kinds of conductive electrodes.
Above-mentioned preparation method, the described electrode of step 4 is sealed electrode and Graphene upper surface in case of necessity.
A kind of method of utilizing said apparatus to measure strain; It is in body surface to be measured with the said apparatus close attachment; Monitoring is communicated with the ohmmeter of Graphene pair of electrodes, when strain takes place in measured surface, and resistance generation significant change; Resistance variations and strain are linear, can the quantitative measurment strain after the demarcation.
A kind of method of utilizing said apparatus to carry out motion-sensing and monitoring; It is that said apparatus is adhered to motion thing surface; Skin surface like people's limbs; Can monitor the synchronous variation of ohmmeter during limb motion, can set up motion and resistance variations corresponding relation, then through resistance variations monitoring motion; Also can be with a flexible apparatus that is equipped with many Graphenes at different directions; Or a plurality of simple flexible apparatus adhere to same moving region; Different to electrode on the resistance variations of observation different directions; Can set up each the thin motion of component units and relation of monitoring resistor seen of moving object, then through a plurality of changes in resistance monitoring motion details.
The strain measurement and the motion sensor means that the present invention is based on Graphene have following advantage and effect:
1. apparatus of the present invention, the preparation method is simple, is suitable for large-scale production such as surface mount.
2. the device that obtains of the inventive method, Stability Analysis of Structures, easy to use, flexible.
3. device wide adaptability of the present invention can be used for various environment and textured surface.
4. device of the present invention is little to the testee influence, can accomplish contactless measurement, is fit to the strain measurement and the biological motion monitoring of special circumstances.
Description of drawings:
Fig. 1 is a typical structure synoptic diagram of the present invention.Figure 1A is the flexible sensing device (1 is that flexible substrates, 2 is that Graphene band, 3 and 4 is termination electrode among the figure) that single Graphene band constitutes; Figure 1B is that four Graphene bands are transferred to the flexible sensing device (1 is that flexible substrates, 2 is that Graphene band, 3 and 4 is termination electrode among the figure) that constitutes on the same flexible substrates; Laterally Graphene band (5) measured X direction strain, vertically Graphene band (2) is measured the Y direction strain of diverse location.
The resistance that Fig. 2 obtains on the stretching and the compressive strain surface of alternation for similar Fig. 1 device is variation relation in time;
Fig. 3 is the strain and the resistance relation of similar Fig. 1 device normalization;
Fig. 4 is that resistance was with upper arm ancon detection of motion signal after similar Fig. 1 device attached to people's upper arm ancon skin surface.Wherein the t1 district is slow crooked upper arm signal, t2, t4 district for the medium speed crooked-stretch flat upper arm signal, t3, t5 district be crooked for fast-stretch and put down the upper arm signal.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated, but the present invention is not limited to following instance.
Method described in the following embodiment like no specified otherwise, is conventional method; Said reagent and material etc. like no specified otherwise, all can obtain from commercial sources.
The first step is made the Graphene strain gauge means like Figure 1A
1. chemical vapor deposition Graphene: with 25 micron thick Copper Foils is substrate, and it is rectangular that Copper Foil is cut to 0.5cm*10cm, keeps 1000 ℃ of growth temperatures; Feed methane and hydrogen, gas flow is methane 25sccm, hydrogen 10sccm; Grow after 15 minutes; Close methane, under the protection of 10sccm hydrogen gas stream, be cooled fast to room temperature, on copper, obtain the grapheme material that the number of plies is the 1-2 layer.
2. Graphene is transferred to dimethyl silicone polymer (PDMS) flexible substrates: the copper sheet surface that will be coated with Graphene is coated with PDMS solution; Place the 0.1M ferric chloride solution to soak copper sheet after the solvent evaporates; After 24 hours, copper dissolves fully, obtains floating on the Graphene-PDMS layer on the solution.
3. be coated with conductive silver glue at two ends, the long limit of Graphene, and draw lead, baking and curing.
4. with sealing silica gel Graphene two ends silver electrode is sealed.
Second step, the test of Graphene strain gauge means
With above-mentioned Graphene device tight adhesion in frosting; Electrode is connected ohmmeter; When plastics are carried out concavo-convex bending; The surface receives tensile strain and compressive strain successively, can see tangible square wave type resistance variations curve (accompanying drawing 2) from ohmmeter, and the peak-to-valley height difference of this waveform is directly proportional with the strain size.
The Graphene preparation is according to the method for embodiment 1.
Substrate uses polymethylmethacrylate (PMMA) to substitute PDMS; Graphene is shifted from copper; It is transferred on polyethylene terephthalate (PET) plastic-substrates: the copper sheet surface that will be coated with Graphene is coated with PMMA solution again, places the 0.1M ferric chloride solution to soak copper sheet after the solvent evaporates, after 24 hours; Copper dissolves fully, obtains floating on the Graphene-PMMA band on the solution; This band is attached in the PET substrate of processing strip in advance, obtains being attached at the Graphene of PET substrate then with acetone flush away PMMA.
Grow the two ends, limit with magnetic control ion sputtering gold electrode (5nm titanium/30nm gold) at Graphene, and draw lead.With sealing silica gel the Graphene two end electrodes is sealed protection.
With the PET substrate be connected to can the strain of quantitative measurment directions X through length experiment table, quantitative measurment is done in the resistance-strain of Graphene strain device, the strain that obtains-resistance concerns shown in accompanying drawing 3.Use this device behind this calibration curve to carry out quantitative strain measurement to other surfaces.
Make the Graphene strain gauge means like Figure 1B, step is following
1. as implement method chemical vapor deposition Graphene in the instance 1, difference is for being growth substrate with 0.5cm*10cm and 0.3*3cm Copper Foil.
2. Graphene is transferred to the PET flexible substrates.The copper sheet surface that is coated with Graphene is coated with PMMA solution; Place the 0.1M ferric chloride solution to soak copper sheet after the solvent evaporates; After 24 hours, copper dissolves fully, obtains floating on the Graphene-PMMA band on the solution; Four Graphenes-PMMA band is transferred in the PET substrate cleaning and removing PMMA according to Figure 1B form.
3. be coated with conductive silver glue at two ends, the long limit of Graphene, and draw lead, baking and curing.
4. with sealing silica gel Graphene two ends silver electrode is sealed.
This device is attached to deformation to be measured surface can be measured the strain of diverse location directions X, Y direction simultaneously.
Prepare the Graphene strain gauge means with method in the embodiment 1, the flexible device that obtains is pasted on people's upper arm ancon inside skin, the motion ancon can observe significantly, the change in electric (like Fig. 4) of different characteristic.Wherein the t1 district is slow crooked upper arm signal, t2, t4 district for the medium speed crooked-stretch flat upper arm signal, t3, t5 district be crooked for fast-stretch and put down the upper arm signal.Explain that this device can be used for motion monitoring significantly.
Embodiment 5
Method is similar with embodiment 2, and difference is that the Graphene two ends are with magnetic control ion sputtering 50nm aluminium electrode, the measurement device strain after sealing.Strain is 1% o'clock, and resistance variations is 5.8%.
Embodiment 6
Method is similar with embodiment 2, and difference is that the Graphene two ends are with hot evaporation coating method vapor deposition 10nm copper electrode, the measurement device strain after sealing.Strain is 1% o'clock, and resistance variations is 6.4%.
Embodiment 7
Method is similar with embodiment 2, and difference is that the Graphene two ends are with magnetic control ion sputtering method sputter 300nm indium tin oxide (ITO) electrode, the measurement device strain after sealing.Strain is 1% o'clock, and resistance variations is 5.6%.
Embodiment 8
The Graphene preparation is according to the method for embodiment 1.
Transfer substrate is used poly tetrafluoroethylene: the copper sheet surface that will be coated with Graphene is coated with PMMA solution, places the 0.1M ferric chloride solution to soak copper sheet after the solvent evaporates, and after 24 hours, copper dissolves fully, obtains floating on the Graphene-PMMA band on the solution; This band is attached on the poly tetrafluoroethylene, uses acetone flush away PMMA then.With magnetic control ion sputtering chromium-gold electrode (5nm chromium/25nm gold), and draw lead at the Graphene two ends.With sealing silica gel the Graphene two end electrodes is sealed protection.The strain measurement result, strain is 1% o'clock, resistance variations is 4.5%.
Embodiment 9
The Graphene preparation is according to the method for embodiment 1.
Transfer substrate is used polyethylene film: the copper sheet surface that will be coated with Graphene is coated with PMMA solution, places the 0.1M ferric chloride solution to soak copper sheet after the solvent evaporates, and after 24 hours, copper dissolves fully, obtains floating on the Graphene-PMMA band on the solution; Magnetron sputtering titanium-Jin termination electrode is attached at the polyethylene film correspondence position with the Graphene band then on polyethylene film.The strain measurement result, strain is 1% o'clock, resistance variations is 6.1%.
Claims (10)
1. one kind based on the strain measurement of Graphene or the device of motion-sensing; It is characterized in that: it is in the substrate of flexible insulation, to be combined with one or more layers graphene film layer; The two ends of graphene film layer are drawn with electrode and are connected ohmmeter; This device is combined closely in testee surface, or a plurality of these devices are combined closely to measure this testee surface strain variations in the testee surface or carry out motion-sensing.
2. device according to claim 1; It is characterized in that: described flexible insulation substrate is the macromolecule flexible polymeric materials, like tygon, PVC, teflon, polypropylene, polyethylene terephthalate, polymethylmethacrylate or dimethyl silicone polymer; Perhaps be composite and flexible material, inorganic fexible film or the gel rubber material that the surface of stability is arranged.
3. device according to claim 1 is characterized in that: described electrode is gold, silver, copper, chromium, titanium, aluminium or platinum, or other is like the film of high conductivity such as indium tin oxide.
4. device according to claim 1 is characterized in that: graphene layer is the band or the lines of aspect ratio.
5. device according to claim 1 is characterized in that: many Graphene bands are combined closely on same flexible substrates with different angles, and every paired extraction electrode in Graphene band two ends makes a device measure the strain or the motion of different directions simultaneously;
Device according to claim 1 is characterized in that: a plurality of these devices are connected in series, and with the resistance variations signal that obtains to strengthen, improve and measure sensitivity.
6. device according to claim 1 is characterized in that: a plurality of independently these flexible apparatus are used stacked system, put, combine closely in same measured surface with the different angles shop, to obtain the strain or the movable information of different directions.
7. method for preparing said strain measurement of claim 1 or motion sensor means, it may further comprise the steps:
The substrate that step 1. prepares to be used to grow Graphene is prefabricated into required form, cleans, then oven dry; Behind the growth Graphene, be reprocessed into required form; Step 2. deposits Graphene on growth substrate.
8. representative condition is: with 25 micron copper foils is substrate, keeps 1000 ℃ of growth temperatures, feeds methane and hydrogen; Gas flow is methane 25sccm; Hydrogen 10sccm grew after 15 minutes, closed methane; Under the protection of 10sccm hydrogen gas stream, be cooled fast to room temperature, on copper, obtain the graphene film that the number of plies is the 1-2 layer;
Step 3. is transferred to graphene film on the required flexible substrates, can pass through repeatedly transfer method and in same substrate, lay many Graphenes; Typical transfer method is: have the copper foil surface of Graphene to be coated with PMMA glue in growth earlier, the graphene layer on copper surface and PMMA layer are adhered to; Place the 0.1M ferric chloride solution to soak 24 hours Copper Foil, erode Copper Foil; The graphene film that is combined with PMMA directly gets into step 4 and draws circuit, maybe this film is attached on other flexible substrates again and uses; Step 4. prepares electrode at Graphene band two ends, and draws circuit.
9. preparation method according to claim 8 is characterized in that: the Graphene growing method described in the step 2 is chemical vapor deposition, plasma reinforced chemical vapour deposition or metal surface epitaxial growth method.
10. preparation method according to claim 8; It is characterized in that: the method that step 4 prepares electrode is directly to be coated with conducting resinl; Or the standard of use silk-screen printing technique, or ion sputtering, electron beam evaporation, hot vapor deposition or magnetron sputtering equal vacuum coating process deposit all kinds of conductive electrodes.
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