CN102957994A - Graphene film speaker and preparation method thereof - Google Patents
Graphene film speaker and preparation method thereof Download PDFInfo
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- CN102957994A CN102957994A CN2012104169630A CN201210416963A CN102957994A CN 102957994 A CN102957994 A CN 102957994A CN 2012104169630 A CN2012104169630 A CN 2012104169630A CN 201210416963 A CN201210416963 A CN 201210416963A CN 102957994 A CN102957994 A CN 102957994A
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Abstract
The invention discloses a graphene film speaker, which comprises a piezoelectric film, wherein one to four layers of grapheme films are respectively arranged at each of the two sides of the piezoelectric film in a bonding way, and two electrodes are connected onto the graphene film. The invention also discloses a preparation method thereof. The graphene film is prepared by a CVD (Chemical Vapor Deposition) method, and a heat release adhesive tape is used as an aid to be transferred to the piezoelectric film, so that the quality and integrity of the graphene film are ensured, and thus the excellent conductivity of the graphene film electrode is ensured, and further the lower power consumption of the graphene film speaker is ensured. The graphene film electrode prepared by the method is more uniform, therefore, the sound pressure is uniform, so that the sound quality is strongly guaranteed. The graphene film speaker generates vibration more easily under the same driving voltage. The graphene film speaker has very high light transmittance, can be used in an electronic device with high light transmittance, and can also be used in a flexible electronic device.
Description
Technical field
The present invention relates to a kind of film speaker and preparation method thereof, more specifically, relate to a kind of Graphene that uses as film speaker of electrode and preparation method thereof.Belong to new material and electric communication technique field.
Background technology
Loud speaker is the equipment that can convert the electrical signal to voice signal.In history, various loud speakers appearred once, for example: dynamic speaker, electromagnetic loudspeaker, crystal speaker, electrostatic loudspeaker etc.In recent years, for satisfying the requirement light and handy to electronic installation, people have researched and developed film speaker.Thereby film speaker utilizes inverse piezoelectric effect that the signal of telecommunication is changed into mechanical oscillation and makes audio reproduction.So-called inverse piezoelectric effect refers to that deformation will occur these dielectrics when when some polarization of dielectric direction applies electric field, and after electric field removed, dielectric deformation also disappeared thereupon, and this phenomenon is called inverse piezoelectric effect.
That summarizes says, film speaker comprises three parts: piezoelectric membrane, and described piezoelectric membrane can mechanically vibrate under the effect that exchanges (AC) voltage; The conducting film electrode is attached on the both sides of piezoelectric membrane; Extraction electrode, described electrode with interchange (AC) voltage transmission of external power source supply to the conducting film electrode.When will the alternating voltage corresponding with voice signal being connected to electrode, piezoelectric membrane will produce vibration under the effect of voltage, thus producing sound.In the film speaker of conventional art, described conducting film generally adopts conductive polymer membrane PEDOT:PSS.Because conductive polymer membrane has high conductivity and lightweight, once once is being subject to people's favor.Yet the compatibility of this conducting polymer and piezoelectric membrane is bad, can not evenly be coated on the piezoelectric membrane.The lack of homogeneity of the thickness of conductive polymer membrane, this is so that the quality that acoustic pressure becomes inhomogeneous and reduced sound.In addition, conducting polymer has chemical resistance and moisture resistance is relatively poor, and its sound pressure characteristic in being lower than the bass zone of 400Hz is also unsatisfactory.
Graphene is a kind ofly to be the cancellated carbonaceous novel film material of hexagon by the monolayer carbon atomic arrangement.It is to be found in 2004 by the strong K of the peace moral of Univ Manchester UK sea nurse (Andre K.Geim) etc., and owing to this discovery has been awarded Nobel Prize in physics in 2010.The characteristic of Graphene maximum be the movement velocity of its electronics reached the light velocity 1/300, lower than copper or silver so Graphene has superpower conductivity considerably beyond the movement velocity of electronics in general conductor, be the present material of resistivity minimum in the world.The graphene film loud speaker is exactly the conductivity of utilizing Graphene superpower, is coated in the loud speaker that the both sides of piezoelectric membrane utilize inverse piezoelectric effect to be made as the conducting film electrode.When the Graphene electrodes on the piezoelectric membrane was passed to alternating current, the internal charge of piezoelectric membrane externally shook under the effect of the attraction of electric field and repulsive force, thereby the signal of telecommunication is changed into voice signal.Accompanying drawing 2 has been showed the operation principle of graphene film loud speaker.
The researcher of South Korea Seoul national university has driven a kind of graphene film formula loud speaker altogether, (Keun-Young Shin, Jin-Yong Hong and Jyongsik Jang, Flexible and transparent graphene films as acoustic actuatorelectrodes using inkjet printing[J] .Chem.Commun., 2011,47,8527 – 8529.) utilize ink-jet printing process and gas phase deposition technology, with graphene oxide at polyvinylidene fluoride (Poly vinylidene Fluoride, PVDF) deposit film forming on the material, then pass through the method for reduction, the graphene oxide film is reduced to graphene film, goes out the graphene film loud speaker with graphene film as electrode fabrication.The graphene film loud speaker of the method preparation has obtained the frequency response from hundreds of to a few KHz relative broad ranges, but also there are many weak points: 1. because there is larger difference in the surface energy of graphene oxide and PVDF material, the inhomogeneous of deformation and thickness change occurs in membrane electrode under capillary effect, and then cause the wafer speaker acoustic pressure inhomogeneous, thereby destroyed the tonequality of graphene film loud speaker.2. because the thin slice of the graphene oxide of graphene oxide suspension only has tens microns, and only after being reduced to Graphene, could conduct electricity, graphene film forms by micron-sized thin slice overlap joint, therefore membrane electrode has higher resistance, square resistance is up to thousands of ohm, and then adds the power consumption that has increased wafer speaker.3. the graphene film of preparation is thicker, and up to 15-20nm, so the transmitance of graphene membrane electrode is lower, and the transparency of graphene film loud speaker is relatively poor.
Summary of the invention
The objective of the invention is provides a kind of graphene film formula loud speaker and preparation method thereof for overcoming above-mentioned the deficiencies in the prior art.
For achieving the above object, the present invention adopts following technical proposals:
A kind of graphene film formula loud speaker, it comprises piezoelectric membrane, all is bonded with 1-6 layer graphene film in the both sides of piezoelectric membrane, is connected with two electrodes at graphene film.
Preferred 1-4 layer graphene film, further preferred 4 layers.The graphene film number of plies of the both sides of piezoelectric membrane can be identical, also can be different.
A kind of preparation method of graphene film formula loud speaker comprises the steps:
(1) adopt the method for chemical vapor deposition (CVD) at metal substrate preparation one deck graphene film;
(2) discharge adhesive tape with adhering to one deck heat on this graphene film surface, as the protective layer of graphene film;
(3) with removing this metal substrate with the solution of the metal generation chemical reaction of metal substrate;
(4) heat is discharged adhesive tape and graphene film and adhere on the piezoelectric membrane, guarantee that graphene film fully contacts with piezoelectric membrane, stay bubble in the middle of avoiding;
Heat release adhesive tape is removed in the piezoelectric membrane heating that (5) will be stained with heat release adhesive tape and graphene film, obtains one-sided piezoelectric membrane with graphene film;
(6) repeating step (2)-(5) adhere to graphene film the opposite side of piezoelectric membrane, obtain bilateral with the piezoelectric membrane of graphene film;
(7) graphene film at piezoelectric membrane picks out two extraction electrodes, has just obtained graphene film formula loud speaker.
Described metal substrate is Cu or Ni paper tinsel, and described chemical solution is FeCl
3Solution.Described FeCl
3The concentration range of solution is 0.1-2mol/L.
Described chemical gaseous phase depositing process catalytic growth Graphene, growth temperature is 800-1100 ℃, utilizes the mist of one or both gases in methane, the acetylene as carbon source, and throughput is 10-300sccm, utilize hydrogen as assist gas, throughput is 10-200sccm; The growth time of giving birth to Graphene is 10-60min.
Described heat discharges the temperature of adhesive tape forfeiture viscosity at 40-90 ℃.
Graphene film selects film laminator to finish with the adhesion process that heat discharges adhesive tape in the described step (2), and the adhesion Speed Setting is 10-50cm/min; Need shilling heat to discharge an end in contact of adhesive tape and graphene film during adhesion, then begin slowly to advance to the other end from contact jaw.Should avoid heat to discharge remaining bubble between adhesive tape and the Cu base graphene film in this process.
Described piezoelectric membrane is that polyvinylidene fluoride (PVDF) is made, and also can be made by the multiple material except polyvinylidene fluoride.
The adhesion of graphene film and piezoelectric membrane adopts film laminator to carry out in the described step (4), and press mold speed is 10-50cm/min; Need an end in contact of shilling Graphene and piezoelectric membrane during adhesion, then begin slowly to advance to the other end from contact jaw.Should avoid heat to discharge remaining bubble between adhesive tape and the piezoelectric membrane in this process.
The piezoelectric membrane that is stained with heat release adhesive tape and graphene film in the described step (5) is placed on the hot plate and toasts, and hot plate temperature is 40-90 ℃, and stoving time is 1-10min.
Continuation repeating step (2)-(5) repeatedly obtained the piezoelectric membrane with the multi-layer graphene film after described step (6) was finished.Described multi-layer graphene film is the 1-6 layer, preferred 4 layers.
The described extraction electrode of described step (7) adopts preferably material of copper strips, silver band, gold ribbon conductivity, or but employing silver coating slurry or spray printing electrically conductive ink are as extraction electrode, the position of extraction electrode is with around the piezoelectric membrane of graphene film, and should expose the edge 1-2mm of piezoelectric membrane, prevent the extraction electrode contact of two faces, cause short circuit.
Graphene film formula loud speaker applies voltage by the graphene membrane electrode to the piezoelectric membrane both sides, this film speaker shows excellent sound pressure characteristic, it is compared with the film speaker of present commercialization, it is thinner more lightly have better flexibility and lower power loss and useful life lasting.Graphene film formula loud speaker only has nanometer grade thickness, has high, the anti-bending of transparency, can stretch, without plurality of advantages such as magnetic, and can cut randomly into various shapes, is placed on the dielectric substrate of arbitrary shape, such as clothes, flag, roof etc.The structure of graphene film formula loud speaker and preparation are very simple, and its appearance will change the mentality of designing of traditional sound equipment acoustics, hew out a new direction in traditional loud speaker industry.
The invention has the beneficial effects as follows:
(1) prepares graphene film with the CVD method, and with heat discharge adhesive tape as secondary transfer to piezoelectric membrane, guarantee quality and the integrality of graphene film, thereby guaranteed the conductivity that graphene membrane electrode is good, and then guaranteed the lower power consumption of graphene film formula loud speaker.
(2) graphene film of the present invention is to shift on the piezoelectric membrane with the form of whole film.Compare with the Graphene electrodes mode of traditional coating electrically conductive polymer or ink-jet printing process preparation, the graphene membrane electrode that this method is made is more even, thereby therefore can make acoustic pressure evenly make tonequality obtain strong assurance.
(3) because graphene film is compared with conducting polymer and is had good chemical resistance and moisture resistance, and graphene film has the Young's modulus suitable with diamond, so graphene film formula loud speaker has more permanent useful life.
(4) because very thin of graphene film, the thickness of single-layer graphene film only is 0.34nm, therefore the thickness of the graphene membrane electrode of the present invention's making only has several nanometers, be far smaller than the thickness of the Graphene electrodes of coating electrically conductive polymer or ink-jet printing process preparation, thereby the graphene film formula loud speaker that this method is made more easily produces vibration under identical driving voltage.
(5) graphene membrane electrode of the present invention's making has very high light transmission rate (accompanying drawing 4), and the Graphene electrodes transmitance for preparing than ink-jet printing process will exceed 10-30%, in addition, because the PVDF piezoelectric membrane itself has higher transmitance.Therefore the graphene film formula loud speaker of the present invention's making has the transparency (accompanying drawing 3) of height, can be used for the electronic installation for high photopermeability needs, and it is placed on display, glass, the picture etc.
(6) graphene membrane electrode of the present invention's making is a complete film, therefore compare with Graphene electrodes, conducting polymer or the ito thin film of ink-jet printing process preparation and have better pliability, the graphene film formula loud speaker that the present invention makes under case of bending, have with flat under same good frequency response (accompanying drawing 7), so the graphene film loud speaker that the present invention makes can be applicable in the flexible electronic device.
Description of drawings
The structure chart of Fig. 1 graphene film formula loud speaker; Wherein 1 is piezoelectric membrane, and 2 is graphene film, and 3 is electrode.
Fig. 2 is graphene film formula speaker operation schematic diagram;
The pictorial diagram of the graphene film formula loud speaker that Fig. 3 embodiment 1 makes;
The corresponding relation figure of the transmitance of Fig. 4 Graphene electrodes and the number of plies; 1,2,3,4 numbers of plies that represent respectively piezoelectric membrane one side wherein.
The corresponding relation figure of the square resistance of Fig. 5 Graphene electrodes and the number of plies;
The frequency response comparison diagram of the graphene film formula loud speaker that Figure 61-4 layer graphene electrode pair is answered and conducting polymer PEDOT:PSS electrode loud speaker; 1,2,3,4 numbers of plies that represent respectively piezoelectric membrane one side wherein.
Fig. 7 Graphene loud speaker is at the comparison diagram of flat and the response of case of bending lower frequency, and what this figure showed is the loud speaker (embodiment 3 preparations) with 3 layer graphene electrodes.Can find out graphene film formula loud speaker under case of bending, have with flat under same good frequency response.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in detail.Embodiment has provided detailed execution mode and concrete operating process, but the present invention is not limited to following examples.
A kind of making of Graphene transparent loudspeaker may further comprise the steps:
(1) the Cu paper tinsel is cut out the constant temperature section of the quartz ampoule of putting into reacting furnace, the air in the quartz ampoule is drained background gas pressure＜100pa with molecular pump system.The closure molecule pumping system passes into hydrogen, and throughput is 100sccm, and furnace temperature is risen to 1050 ℃, will pass into methane behind the Cu paper tinsel annealing 30min, and throughput is set as 25sccm.Behind the reaction 30min, with closing methane, allow quartz ampoule in atmosphere of hydrogen, be cooled to room temperature.
(2) discharge adhesive tape with adhering to one deck heat on the Cu base Graphene film surface, as the protective layer of graphene film.Adhesion process can select film laminator to finish, and the adhesion Speed Setting is 15cm/min.Wherein, to put the temperature of adhesive tape forfeiture viscosity be 80 ℃ to described heat.
The Cu base graphene film that (3) will adhere to one deck heat release adhesive tape is put into the FeCl that concentration is 1mol/L
3Soaking at room temperature in the solution after Cu corrosion fully, discharges adhesive tape with heat and graphene film moves in the clear water to remove remaining FeCl
3, clean fully rear taking-up and dry for subsequent use.
(4) cleaned heat release adhesive tape and graphene film are adhered on the piezoelectric membrane, this process adopts film laminator to carry out, need an end in contact of shilling adhesive tape and piezoelectric membrane during adhesion, then begin slowly to advance to the other end from contact jaw, avoid heat to discharge remaining bubble between adhesive tape and the piezoelectric membrane, press mold speed is 15cm/min.
(5) will being stained with piezoelectric membrane that heat discharges adhesive tape and graphene film, to be placed on temperature be to toast 5min on 80 ℃ the hot plate, discharges the piezoelectric membrane that has just obtained after adhesive tape loses viscosity and Graphene separates with graphene film until heat.It should be noted that hot plate temperature does not surpass the working temperature of piezoelectric membrane, in case surpass, will make the deformation of piezoelectric membrane generation irrecoverability, cause the change of piezoelectric membrane character.
(6) repeat the opposite side that graphene film can be transferred to piezoelectric membrane in (2)-(5), obtain bilateral with the piezoelectric membrane of graphene membrane electrode.
(7) pick out two extraction electrodes around the graphene film of piezoelectric membrane, the extraction electrode material is selected the copper of good conductivity, has just obtained the Graphene transparent loudspeaker behind the extraction electrode.
Can see that from the pictorial diagram of accompanying drawing 3 Graphene loud speakers graphene film formula loud speaker has the extraordinary transparency.
Concrete steps are with embodiment 1, and difference is execution in step (2)-(5) process 4 times,, obtain the piezoelectric membrane with double-layer graphite alkene film on each face for 2 times.As shown in Figure 1, the both sides that obtain piezoelectric membrane respectively are bonded with the graphene film formula loud speaker of 2 layer graphene films.
Concrete steps are with embodiment 1, and difference is execution in step (2)-(5) process 6 times,, obtain the piezoelectric membrane with 3 layer graphene films on each face for 3 times.
Embodiment 4
Concrete steps are with embodiment 1, and difference is execution in step (2)-(5) process 8 times,, obtain the piezoelectric membrane with 4 layer graphene films on each face for 4 times.
Embodiment 5
Concrete steps are with embodiment 1, and difference is execution in step (2)-(5) process 10 times,, obtain the piezoelectric membrane with 5 layer graphene films on each face for 5 times.
Embodiment 6
Concrete steps are with embodiment 1, and difference is execution in step (2)-(5) process 12 times,, obtain the piezoelectric membrane with 6 layer graphene films on each face for 6 times.
The graphene film formula loud speaker that above-described embodiment 1-6 makes is compared with the graphene film formula loud speaker that adopts the ink-jet printing process preparation has obvious advantage:
1. the resistance of its electrode of graphene film formula loud speaker of the present invention's making is hundreds of Ω/ (accompanying drawing 5), and the resistance that adopts its electrode of graphene film formula loud speaker of ink-jet printing process preparation is tens and even K Ω/ up to a hundred, therefore, the Graphene loud speaker of the present invention's making has lower power consumption.
2. the transmitance of its electrode of graphene film formula loud speaker of the present invention's making is at (accompanying drawing 4) more than 90%, and the transmitance of its its electrode of graphene film formula loud speaker that adopts the ink-jet printing process preparation is between 66-92%, and the graphene film formula loud speaker that the present invention makes has better transparency.
3. its frequency response curve of graphene film formula loud speaker (accompanying drawing 6) of the present invention's making is compared more level and smooth with the frequency response curve of the graphene film formula loud speaker that adopts the ink-jet printing process preparation, show that the wafer speaker acoustic pressure that the present invention makes is more stable, tonequality is better.
Claims (10)
1. a graphene film formula loud speaker is characterized in that, it comprises piezoelectric membrane, all is bonded with 1-6 layer graphene film in the both sides of piezoelectric membrane, is connected with two electrodes at graphene film.
2. the preparation method of a graphene film formula loud speaker is characterized in that, comprises the steps:
(1) adopt the method for chemical vapour deposition (CVD) at metal substrate preparation one deck graphene film;
(2) discharge adhesive tape with adhering to one deck heat on this graphene film surface, as the protective layer of graphene film;
(3) with removing this metal substrate with the solution of the metal generation chemical reaction of metal substrate;
(4) heat is discharged adhesive tape and graphene film and adhere on the piezoelectric membrane, guarantee that graphene film fully contacts with piezoelectric membrane, stay bubble in the middle of avoiding;
Heat release adhesive tape is removed in the piezoelectric membrane heating that (5) will be stained with heat release adhesive tape and graphene film, must be with the piezoelectric membrane of graphene film;
(6) repeating step (2)-(5) adhere to graphene film the opposite side of piezoelectric membrane, obtain the piezoelectric membrane with graphene film;
(7) graphene film at piezoelectric membrane picks out two extraction electrodes, has just obtained graphene film formula loud speaker.
3. preparation method as claimed in claim 2 is characterized in that, described metal substrate is Cu paper tinsel or Ni paper tinsel, and described chemical solution is FeCl
3Solution.
4. preparation method as claimed in claim 2, it is characterized in that, described chemical gaseous phase depositing process catalytic growth Graphene, growth temperature is 800-1100 ℃, utilize the mist of one or both gases in methane, the acetylene as carbon source, throughput is 10-300sccm, utilizes hydrogen as assist gas, and throughput is 10-200sccm; The growth time of giving birth to Graphene is 10-60min.
5. preparation method as claimed in claim 2 is characterized in that, described heat discharges the temperature of adhesive tape forfeiture viscosity at 40-90 ℃.
6. preparation method as claimed in claim 2 is characterized in that, graphene film selects film laminator to finish with the adhesion process that heat discharges adhesive tape in the described step (2), and the adhesion Speed Setting is 10-50cm/min; Need shilling heat to discharge an end in contact of adhesive tape and graphene film during adhesion, then begin slowly to advance to the other end from contact jaw.
7. preparation method as claimed in claim 2 is characterized in that, the adhesion of graphene film and piezoelectric membrane adopts film laminator to carry out in the described step (4), and press mold speed is 10-50cm/min; Need an end in contact of shilling adhesive tape and piezoelectric membrane during adhesion, then begin slowly to advance to the other end from contact jaw.
8. preparation method as claimed in claim 2 is characterized in that, the piezoelectric membrane that is stained with heat release adhesive tape and graphene film in the described step (5) is placed on the hot plate and toasts, and hot plate temperature is 40-90 ℃, and stoving time is 1-10min.
9. preparation method as claimed in claim 2 is characterized in that, continuation repeating step (2)-(5) repeatedly obtained the piezoelectric membrane with the multi-layer graphene film after described step (6) was finished.
10. preparation method as claimed in claim 2, it is characterized in that, the described extraction electrode of described step (7) adopts preferably material of copper strips, silver band, gold ribbon conductivity, or but employing silver coating slurry or spray printing electrically conductive ink are as extraction electrode, the position of extraction electrode is with around the piezoelectric membrane of graphene film, and should expose the edge 1-2mm of piezoelectric membrane, and prevent the extraction electrode contact of two faces, cause short circuit.
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| CN107318076A (en) * | 2017-06-26 | 2017-11-03 | 上海集成电路研发中心有限公司 | A kind of MEMS acoustic sensors based on graphene and preparation method thereof |
| CN108281376A (en) * | 2018-01-22 | 2018-07-13 | 南京工业大学 | A kind of preparation method of semiconductor devices |
| CN108513245A (en) * | 2018-05-10 | 2018-09-07 | Oppo广东移动通信有限公司 | Electroacoustic component, electronic equipment and its manufacturing method |
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