CN108862246A - A kind of adjustable nanoscale sonic generator of tone color - Google Patents
A kind of adjustable nanoscale sonic generator of tone color Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B06—GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS IN GENERAL
- B06B—METHODS OR APPARATUS FOR GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS OF INFRASONIC, SONIC, OR ULTRASONIC FREQUENCY, e.g. FOR PERFORMING MECHANICAL WORK IN GENERAL
- B06B1/00—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
- B06B1/02—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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Abstract
The invention discloses a kind of adjustable nanoscale sonic generators of tone color, it is lower than the substrate of 200W/mK, the sound generating membranes being laid in substrate including thermal conductivity, and two tone currents input elargol electrode and electrical signal input units, two elargol electrodes are separately positioned on the both ends of sound generating membranes, sound generating membranes, two elargol electrodes and electrical signal input unit series connection forming circuit；Sound generating membranes are graphene film, with a thickness of 60nm, 2.0~2.2g/cm of density is not more than3Between, it is crosslinked between graphene layer, the degree of cross linking has excellent electric heating property and thermal conductivity, can effectively cause the temperature vibration of air at film in 1-5%, the graphene film.The microphone device sound quality is good, and sound articulation is high, and take-over point among the thermal conductivity and design free standing structure film by regulating and controlling film to adjust the waveform of sound excitation, and then adjusts tone color.
Description
Technical field
The present invention relates to high-performance nano material and preparation method thereof more particularly to a kind of adjustable nanoscale sound waves of tone color
Generator.
Background technique
2010, two professor Andre GeiM and Konstantin Novoselov of Univ Manchester UK because
It is successfully separated out stable graphene for the first time and obtains Nobel Prize in physics, has started the upsurge that graphene is studied in the whole world.
Graphene has excellent electric property (electron mobility is up to 2 × 105cM2/Vs at room temperature), performance (5000W/ outstanding
(MK), extraordinary specific surface area (2630M2/g), Young's modulus (1100GPa) and breaking strength (125GPa).Graphene is excellent
Different electrical and thermal conductivity performance is well beyond metal, while graphene has the advantages that corrosion-and high-temp-resistant, and its good machinery
Performance and lower density more allow it to have the potentiality in thermo electric material field substituted metal.
The graphene film of macroscopic view assembling graphene oxide or graphene nanometer sheet is the main application of nanoscale graphite alkene
Form, common preparation method are suction methods, scrape embrane method, spin-coating method, spray coating method and dip coating etc..At further high temperature
Reason, can repair the defect of graphene, can effectively improve the electric conductivity and thermal conductance of graphene film, can be widely applied to
Sounding, acoustic detection, smart phone, intelligence are with oneself in the accompanied electronics equipment such as hardware, tablet computer, laptop.
But because of the presence of edge defect, in addition active force is weak between graphene layer, the graphene film one that high temperature sintering is crossed
As intensity it is all less high, be less than 100MPa, be unfavorable for its practical application.In addition, cross-linked structure and diamond knot between graphene layer
Structure is similar, does not damage to thermally conductive, will not seriously affect the heating conduction of graphene film.
So far, graphene film has begun PI base graphene film, the change applied to microphone device, such as laser preparation
Learn the graphene film of reduction.But both of the above film has inevitable defect, first, fault of construction is big, heating rate
Slowly；Second, thickness is very high, cooling rate is slow, and the clarity of sounding is poor thus；Third, film temperature tolerance is poor, sound equipment is adjusted
It is poor to spend；Most of all, the above film cannot all adjust tone color, to not have discrimination to sound.In view of the above problems, this
Patent design nanometer thickness cross-linked graphene film.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of adjustable nanoscale sonic generator of tone color.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of adjustable nanoscale sonic generator of tone color,
Including two copper billets, sound generating membranes and electrical signal input unit, the both ends of sound generating membranes are overlapped in copper billet table
Face, two copper billets are connected with the positive and negative anodes of electrical signal input unit respectively；Sound generating membranes are graphene film, with a thickness of little
It between 60nm, 2.0~2.2g/cm3 of density, is crosslinked between graphene layer, the degree of cross linking passes through in 1-5%, graphene film with lower section
Method is prepared：
(1) graphene oxide is configured to concentration is 0.5-10ug/mL graphene oxide water solution, filters film forming；
(2) graphene oxide membrane filtered in substrate will be attached to be placed in closed container, 80-100 degree HI high temperature is the bottom of from
Up fumigate 0.1-1h in portion；
(3) by the solid transfer agent even application of thawing in redox graphene film surface, and it is slowly cold at room temperature
But, until film and substrate separate；
(4) to step 3, treated that redox graphene film heats so that the distillation of solid transfer agent or
Volatilization；
(5) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of Titanium, molybdenum or cobalt etc.
Metal, 30% of mole no more than carbon atom mole in graphene film of the metal nanoparticle of sputtering.
(6) there is the graphene film of metal to carry out chlorination processing sputtering under 800-1200 degrees Celsius, metal nanoparticle with
Chloride form loss；
(7) graphene film after chlorination is placed in high temperature furnace, is warming up to 1500 degrees Celsius with 5-20 centigrade per minute, so
2000 degree of high temperature are warming up to 2-5 centigrade per minute afterwards, obtain the graphene film of interlayer crosslinking.
Further, substrate of the thermal conductivity lower than 200W/mK is selected from polymeric substrates, silicon base.
Further, solid transfer agent is selected from following substance, such as paraffin, naphthalene, arsenic trioxide, camphor, sulphur, drop ice
The small molecule solid matter not soluble in water that piece alkene, rosin etc. can distil or volatilize under certain conditions.
Further, the sublimation temperature of solid transfer agent will be controlled at 320 degree or less.
Further, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in the environment of 0.5-10%, time 0.1-4h.
Further, the both ends of sound generating membranes are overlapped in the upper surface of copper billet by the following method：The table on copper billet
Face sprays ethyl alcohol, and the end of sound generating membranes is attached in liquid surface, ethanol evaporation.
Further, the both ends of sound generating membranes also pass through encapsulating material and are further secured to copper block surface, sound wave hair
Raw film is directly contacted with copper block surface.
The beneficial effects of the present invention are：The mode of present invention solid transfer first, obtains ultra-thin graphene film, is device
The high resistance of part lays the foundation；Further by (1 DEG C/min) processing that slowly heats up, increase graphene membrane surface fold, extension
The area of graphene film in unit space；Then 2000 DEG C are set with 10 DEG C/min heating, to remove the overwhelming majority inside graphene
Atom defect, but do not restore stacked structure inside graphene.Further by ultra-thin graphene membrane surface splash-proofing sputtering metal particle,
Under high temperature, metallic and graphite alkene reaction form metal carbides；Then metal carbides are formed under the action of chlorine
Metal chloride and loss, meanwhile, carbon structure changes to diamond lattic structure, greatly improves film strength (reaching 7-20GPa)
And thermal stability, 2000 degree of high-temperature process so that graphene film structure obtains the recovery of high degree, but will not influence interlayer
Cross-linked structure and it not will form AB packed structures.The present invention sacrifices the partially electronically conductive heating conduction of graphene film, and interlayer is handed over
It is coupled structure and introduces graphene film interlayer, graphene film strength is greatly improved, by 80 times of its strength enhancing or more.This film is answered
For acoustic detection, there is following advantage：First, membrane structure is perfect, structure and accumulation defect are few, and conductivity is high, heating speed
Degree is fast；Second, film thickness is in 60nm hereinafter, thermal conductivity is high, rapid heat dissipation；The above graphene film temperature rate is fast, determines
This film has fabulous sound quality, and sound articulation is high.Third, graphene film defect is few, internal crosslinking, thermal stability is good, can
To be resistant to 520 degree in air of high temperature, sonority controllability is good；Fourth, graphene film thermal conductivity is high, sounding voltage is lower；
Fifth, being designed by structure, this film can be come by regulating and controlling the thermal conductivity of film and designing take-over point among free standing structure film
The waveform of sound excitation is adjusted, and then adjusts tone color.
Detailed description of the invention
Fig. 1 is 2000 degrees Celsius of no cross-linked graphene film treated Raman map.
Fig. 2 is 2000 degrees Celsius of cross-linked graphene film treated Raman map.
The transmission map that Fig. 3 is handled for 2000 degrees Celsius of no cross-linked graphene film.
Fig. 4 is the transmission map of 2000 degrees Celsius of cross-linked graphene film processing.
Fig. 5 is that the tensile strength of 2000 degrees Celsius of cross-linked graphene film processing tests map.
Fig. 6 is the heating temperature lowering curve of the obtained graphene film of embodiment 1.
Fig. 7 is the T=1s moment, graphene film along two electrodes temperature curve in the straight direction.
Fig. 8 is that embodiment 4 has the graphene film of 3 heat derives points in the temperature curve at T=1s moment.
Specific embodiment
Embodiment 1：
(1) graphene oxide is configured to concentration is 0.5ug/mL graphene oxide water solution, with hydrophilic polytetrafluoroethylmicroporous
Film is that substrate filters film forming.
(2) graphene oxide membrane for being attached at hydrophilic polytetrafluoroethylmicroporous film is placed in closed container, 80 degree of HI high temperature from
Up fumigate 1h in bottom.
(3) use the methods of vapor deposition, curtain coating by the solid transfer agent camphor even application of thawing in redox graphene film
Surface, and Slow cooling at room temperature, film and substrate separation.
(4) graphene film that solid transfer agent obtained above supports slowly is vapored away into solid transfer agent under 40 degree,
Obtain the graphene film of independent self-supporting.
(5) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of Titanium.It is splashed by control
Parameter is penetrated, the mole of the metal nanoparticle finally sputtered is 28.6% of carbon atom mole in graphene film.
There is the graphene film of metal to carry out chlorination processing sputtering under (6) 1200 degrees Celsius, so that titanium nanoparticle is with chlorine
Compound form loss.Specifically, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in 0.5% environment, time 4h.
(7) 2000 degree of high-temperature process of the graphene film after chlorination, 2000 degree of pyroprocess temperature-rise periods are as follows：1500 is Celsius
Degree is hereinafter, 20 centigrade per minutes；1500 degrees Celsius or more, 5 centigrade per minutes；Obtain the graphene film with a thickness of 59nm.
Comparison diagram 1,2 has the graphene film of numerous cross-linked structures to have stronger sp3Bonded peak (the 1360cm of carbon-1), pass through
ID/IG area ratio measures, and (degree of cross linking is sp to the degree of cross linking3Content-mass percent of carbon) it is 4.8%；Fig. 3,4, have
The graphene film electronic diffraction striped interlamellar spacing of cross-linked structure is smaller than normal graphene film electronic diffraction interlamellar spacing.Such as Fig. 5 institute
Show, prepared graphene film intensity is 7GPa, it is ensured that its thermal stability.The density of graphene film is 2.0g/cm3。
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
2×2cm2The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of 10V power supply respectively, and
With the temperature change in temperature-control senser measurement graphene film middle position, this graphene film is under atmospheric environment, in the straight of 10V
Galvanic electricity pressure, it is only necessary to just reach within 0.5 second 518 DEG C of equilibrium temperature, and after powering off, due to the heat transfer that graphene film is excellent
Property, the temperature of film are just dropped in 0.5 second close to room temperature, as shown in Figure 6.To the T=1s moment, obtained using infrared detecting set thin
Film surface temperature profile, in the straight direction along two electrode institutes, centre is high, both ends bottom, as shown in Figure 7 for the graphene film.
The waveform of this film different temperatures represents film to air pulsation mode, air vibration, and shape is caused in heating and cooling process
At the sound wave of corresponding waveform.Therefore, sound can be changed by adjusting the thermal conductivity (thermal conductivity is higher, and waveform is more flat) of graphene
Wave waveform, to obtain different tone colors.
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of electrical signal input unit respectively, structure
At nanoscale sonic generator of the present invention.It, can very exothermic in applied voltage due to film conductivity height
Heating, withdraws applied voltage, and film is because the reason of thermal conductivity is good and thinner thickness, heat dissipation very high speed, the two are common
Effect, allows the quick heating and cooling of film, so as to cause the temperature vibration of air at film, thus sounding.Therefore, pass through
In addition the secondary load of the DC voltage of 10V loads specified input audio signal, adjust the voltage integrally inputted and variation frequency
Rate can obtain determining air temperature vibration amplitude, i.e. pitch；Air temperature vibration can be adjusted by adjusting frequency input signal
Frequency, and then the frequency shift of sounding, issue different sound；And the tone color of the sonic generator is adjustable.
Embodiment 2：
(1) by graphene oxide be configured to concentration be 10ug/mL graphene oxide water solution, using PC film be substrate suction filtration at
Film.
(2) graphene oxide membrane for being attached at PC film is placed in closed container, 100 degree of HI high temperature are up fumigated from bottom
0.1h。
(3) use the methods of vapor deposition, curtain coating by the solid transfer agent naphthalene even application of thawing in redox graphene film table
Face, and Slow cooling at room temperature.
(4) the slowly volatilization under 80 by the graphene film of solid transfer agent obtained above support, obtains independent self-supporting
Graphene film.
(5) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of Titanium.It is splashed by control
Parameter is penetrated, the mole of the metal nanoparticle finally sputtered is 18.4% of carbon atom mole in graphene film.
There is the graphene film of metal to carry out chlorination processing sputtering under (6) 800 degrees Celsius, so that titanium nanoparticle is with chlorination
Object form loss.Specifically, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in 10% environment, time 0.1h.
(7) 2000 degree of high-temperature process of the graphene film after chlorination, specially：1500 degrees Celsius hereinafter, 5 degrees Celsius every point
Clock；1500 degrees Celsius or more, 2 centigrade per minutes；2000 degree of heat preservation 1h；Obtain the graphene film with a thickness of 48nm.
It is tested through Raman, which has the graphene film of numerous cross-linked structures to have stronger sp3The bonded peak of carbon
(1360cm-1), it is measured by ID/IG area ratio, (degree of cross linking is sp to the degree of cross linking3Content-mass percent of carbon) be
1.1%；The graphene film electronic diffraction striped interlamellar spacing of crosslinking structure is smaller than normal graphene film electronic diffraction interlamellar spacing.
Prepared graphene film intensity is 7.6GPa, density 2.0g/cm3。
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
2×2cm2The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of 10V power supply respectively, and
With the temperature change among temperature-control senser measurement graphene film, this graphene film is under atmospheric environment, in the direct current of 10V
Pressure, it is only necessary to just reach within 0.5 second 514 DEG C of equilibrium temperature, and after powering off, due to the heat conductivity that graphene film is excellent, film
Temperature just drop in 0.5 second close to room temperature, to the T=1s moment, infrared detecting set is utilized to obtain film surface temperature distribution
Figure, in the straight direction along two electrode institutes, centre is high, both ends bottom for the graphene film.
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of electrical signal input unit respectively, structure
At nanoscale sonic generator of the present invention.
Embodiment 3：
(1) graphene oxide is configured to concentration is 1ug/mL graphene oxide water solution, with hydrophilic polytetrafluoroethylmicroporous film
It filters and forms a film for substrate.
(2) hydrophilic polytetrafluoroethylmicroporous graphene oxide membrane will be attached to be placed in closed container, 90 degree of HI high temperature are the bottom of from
Up fumigate 0.5h in portion.
(3) use the methods of vapor deposition, curtain coating by the solid transfer agent sulphur even application of thawing in redox graphene film table
Face, and Slow cooling at room temperature.
(4) graphene film that solid transfer agent obtained above supports slowly is volatilized under 120 degree, is obtained independent from branch
The graphene film of support.
(5) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of metallic cobalt, is splashed by control
Parameter is penetrated, the mole of the metal nanoparticle finally sputtered is 15.9% of carbon atom mole in graphene film.
There is the graphene film of metal to carry out chlorination processing sputtering under (6) 1000 degrees Celsius, so that cobalt nanometer particle is with chlorine
Compound form loss.Specifically, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in 5% environment, time 1h.
(7) 2000 degree of high-temperature process of the graphene film after chlorination, specially：1500 degrees Celsius hereinafter, 10 degrees Celsius every point
Clock；1500 degrees Celsius or more, 3 centigrade per minutes；2000 degrees Celsius of heat preservation 0.5h；Obtain the graphene film with a thickness of 28nm.
It is tested through Raman, which has the graphene film of numerous cross-linked structures to have stronger sp3The bonded peak of carbon
(1360cm-1), it is measured by ID/IG area ratio, (degree of cross linking is sp to the degree of cross linking3Content-mass percent of carbon) be
1.9%；The graphene film electronic diffraction striped interlamellar spacing of crosslinking structure is smaller than normal graphene film electronic diffraction interlamellar spacing.
Prepared graphene film intensity is 11GPa, density 2.1g/cm3。
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
2×2cm2The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of 10V power supply respectively, and
With the temperature change among temperature-control senser measurement graphene film, this graphene film is under atmospheric environment, in the direct current of 10V
Pressure, it is only necessary to just reach within 0.5 second 518 DEG C of equilibrium temperature, and after powering off, due to the heat conductivity that graphene film is excellent, film
Temperature just drop in 0.5 second close to room temperature, to the T=1s moment, infrared detecting set is utilized to obtain film surface temperature distribution
Figure, in the straight direction along two electrode institutes, centre is high, both ends bottom for the graphene film.
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of electrical signal input unit respectively, structure
At nanoscale sonic generator of the present invention.
Embodiment 4：
(1) by graphene oxide be configured to concentration be 3ug/mL graphene oxide water solution, using AAO film be substrate suction filtration at
Film.
(2) graphene oxide membrane for being attached at AAO film is placed in closed container, 100 degree of HI high temperature are up smoked from bottom
Steam 0.2h.
(3) use the methods of vapor deposition, curtain coating by the solid transfer agent paraffin even application of thawing in redox graphene film
Surface, and Slow cooling at room temperature.
(4) graphene film that solid transfer agent obtained above supports slowly is volatilized under 200 degree, is obtained independent from branch
The graphene film of support.
(5) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of Titanium, is splashed by control
Parameter is penetrated, the mole of the metal nanoparticle finally sputtered is 25.4% of carbon atom mole in graphene film.
There is the graphene film of metal to carry out chlorination processing sputtering under (5) 1100 degrees Celsius, so that titanium nanoparticle is with chlorine
Compound form loss.Specifically, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in 2% environment, time 2h.
(6) 2000 degree of high-temperature process of the graphene film after chlorination, specially：1500 degrees Celsius hereinafter, 12 degrees Celsius every point
Clock；1500 degrees Celsius or more, 4 centigrade per minutes；2000 degrees Celsius of heat preservation 1h, obtain the graphene film with a thickness of 33nm.
It is tested through Raman, which has the graphene film of numerous cross-linked structures to have stronger sp3The bonded peak of carbon
(1360cm-1), it is measured by ID/IG area ratio, (degree of cross linking is sp to the degree of cross linking3Content-mass percent of carbon) be
2.2%；The graphene film electronic diffraction striped interlamellar spacing of crosslinking structure is smaller than normal graphene film electronic diffraction interlamellar spacing.
Prepared graphene film intensity is 9.6GPa, density 2.0g/cm3。
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
2×2cm2The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of 10V power supply respectively, together
When, a silico briquette is placed in the middle position between two copper billets, and sound generating membranes are directly contacted with silico briquette surface.Then it uses
Temperature-control senser measures temperature change of the graphene film at silico briquette 0.5cm under atmospheric environment, in the DC voltage of 10V
Under, it is only necessary to just reach within 0.5 second 506 DEG C of equilibrium temperature, and after powering off, due to the heat conductivity that graphene film is excellent, film
Temperature just drops in 0.5 second close to room temperature.
A silico briquette is placed in middle position between two copper billets, and sound generating membranes middle position and silico briquette surface are straight
Contact.The DC voltage of two copper billet input 10V obtains the T=1s moment using infrared detecting set according to the method described above
Film surface temperature distribution map, in the straight direction along two electrode institutes, temperature curve changes the graphene film, as shown in Figure 8.
Therefore, temperature variation curve can be changed by along linearly increasing heat derives point, to change acoustic waveform, obtained different
Tone color.
Embodiment 5：
(1) graphene oxide is configured to concentration is 10ug/mL graphene oxide water solution, with hydrophilic polytetrafluoroethylmicroporous film
It filters and forms a film for substrate.
(2) graphene oxide membrane for being attached at hydrophilic polytetrafluoroethylmicroporous film is placed in closed container, 80 degree of HI high temperature from
Up fumigate 0.8h in bottom.
(3) use the methods of vapor deposition, curtain coating by the solid transfer agent norbornene even application of thawing in reduction-oxidation graphite
Alkene film surface, and Slow cooling at room temperature.
(4) graphene film that solid transfer agent obtained above supports slowly is waved under 60 degree, 2 atmospheric pressure, is obtained
The graphene film of independent self-supporting.
(4) graphene membrane surface with the mode of magnetron sputtering in electronation sprays one layer of metal molybdenum.It is splashed by control
Parameter is penetrated, the mole of the metal nanoparticle finally sputtered is 22.8% of carbon atom mole in graphene film.
There is the graphene film of metal to carry out chlorination processing sputtering under (5) 800 degrees Celsius, so that molybdenum nanoparticle is with chlorination
Object form loss.Specifically, chlorination processing refers to：The graphene film that sputtering has metal nanoparticle, which is placed in chlorine content, is
Heated in 6% environment, time 3h.
(6) 2000 degree of high-temperature process of the graphene film after chlorination, specially：1500 degrees Celsius hereinafter, 7 degrees Celsius every point
Clock；1500 degrees Celsius or more, 2 centigrade per minutes, 2000 degrees Celsius of heat preservation 1h obtain the graphene film with a thickness of 36nm.
It is tested through Raman, which has the graphene film of numerous cross-linked structures to have stronger sp3The bonded peak of carbon
(1360cm-1), it is measured by ID/IG area ratio, (degree of cross linking is sp to the degree of cross linking3Content-mass percent of carbon) be
3.7%；The graphene film electronic diffraction striped interlamellar spacing of crosslinking structure is smaller than normal graphene film electronic diffraction interlamellar spacing.
Prepared graphene film intensity is 9.8GPa, density 2.2g/cm3。
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
2×2cm2The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of 10V power supply respectively, and
With the temperature change among temperature-control senser measurement graphene film, this graphene film is under atmospheric environment, in the direct current of 10V
Pressure, it is only necessary to just reach within 0.5 second 503 DEG C of equilibrium temperature, and after powering off, due to the heat conductivity that graphene film is excellent, film
Temperature just drop in 0.5 second close to room temperature, to the T=1s moment, infrared detecting set is utilized to obtain film surface temperature distribution
Figure, in the straight direction along two electrode institutes, centre is high, both ends bottom for the graphene film.
Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid surface, ethanol evaporation, so that
The both ends of sound generating membranes are overlapped in copper block surface, and two copper billets are connected with the positive and negative anodes of electrical signal input unit respectively, structure
At nanoscale sonic generator of the present invention.
Claims (7)
1. a kind of adjustable nanoscale sonic generator of tone color, which is characterized in that including two copper billets, sound generating membranes, with
And electrical signal input unit, the both ends of sound generating membranes are overlapped in copper block surface, two copper billets input with electric signal single respectively
The positive and negative anodes of member are connected；The sound generating membranes are graphene film, with a thickness of 60nm, 2.0~2.2g/cm of density is not more than3
Between, it is crosslinked between graphene layer, the degree of cross linking is prepared by the following method to obtain in 1-5%, the graphene film：
(1) graphene oxide is configured to concentration is 0.5-10ug/mL graphene oxide water solution, filters film forming.
(2) graphene oxide membrane that will be attached in suction filtration substrate is placed in closed container, and 80-100 degree HI high temperature is past from bottom
Upper stifling 0.1-1h.
(3) by the solid transfer agent even application of thawing in redox graphene film surface, and Slow cooling at room temperature, directly
It is separated to film and substrate；
(4) to step 3, treated that redox graphene film heats, so that the distillation of solid transfer agent or waving
Hair；
(5) graphene membrane surface one layer of Titanium of spraying with the mode of magnetron sputtering in electronation, the metals such as molybdenum or cobalt,
30% of the mole of the metal nanoparticle of sputtering no more than carbon atom mole in graphene film.
(6) graphene film of metal carries out chlorination processing sputtering under 800-1200 degrees Celsius, metal nanoparticle is with chlorination
Object form loss；
(7) graphene film after chlorination is placed in high temperature furnace, is warming up to 1500 degrees Celsius with 5-20 centigrade per minute, then with
2-5 centigrade per minute is warming up to 2000 degree of high temperature, obtains the graphene film of interlayer crosslinking.
2. nanoscale sonic generator as described in claim 1, which is characterized in that substrate of the thermal conductivity lower than 200W/mK is selected
Autohemagglutination polymer substrates, silicon base.
3. nanoscale sonic generator as described in claim 1, which is characterized in that the solid transfer agent, selected from as follows
Substance, such as paraffin, naphthalene, arsenic trioxide, camphor, sulphur, norbornene, rosin etc. can distil or volatilize under certain conditions
Small molecule solid matter not soluble in water.
4. nanoscale sonic generator as described in claim 1, which is characterized in that the sublimation temperature of the solid transfer agent
It controls at 320 degree or less.
5. nanoscale sonic generator as described in claim 1, which is characterized in that the chlorination processing refers to：Sputtering is had
The graphene film of metal nanoparticle, which is placed in the environment that chlorine content is 0.5-10%, to be heated, time 0.1-
4h。
6. nanoscale sonic generator as described in claim 1, which is characterized in that the both ends of sound generating membranes pass through as follows
Method is overlapped in the upper surface of copper billet：Ethyl alcohol is sprayed in copper billet upper surface, the end of sound generating membranes is attached in liquid table
Face, ethanol evaporation.
7. nanoscale sonic generator as described in claim 1, which is characterized in that the both ends of the sound generating membranes are also logical
It crosses encapsulating material and is further secured to copper block surface, sound generating membranes are directly contacted with copper block surface.
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