CN108871547A - A kind of graphene film base low-frequency sound wave detector - Google Patents
A kind of graphene film base low-frequency sound wave detector Download PDFInfo
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- G01H—MEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
- G01H11/00—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties
- G01H11/06—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means
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Abstract
The invention discloses a kind of graphene film base low-frequency sound wave detector, which, for main sensitive detection parts, by assembling design, forms the capacitor by graphene/conductive substrates for the two poles of the earth with high-strength graphite alkene film.Acoustic wave vibrations cause the vibration of graphene film, change the distance between graphene film and conductive substrates, and then cause capacitance variations, generate current signal.This etched drilling of high-strength graphite alkene, vacuum filter film forming, electronation, solid phase transfer, metal spraying, medium temperature carbonization, green gas chlorination, high temperature graphitization and etc. obtain.The film generally graphene-structured, piece interlayer have a large amount of interlayer cross-linked structures.Monolithic film membrane is with a thickness of 20-50nm.This graphene film conductivity is controllable, intensity is adjustable, can be used as low-frequency sound wave sensitive detection parts.
Description
Technical field
The present invention relates to high performance device more particularly to a kind of graphene film base low-frequency sound wave detectors.
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, and (electron mobility is up to 2 × 10 at room temperature5cM2/ Vs), heating conduction (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
Smart phone, intelligence are with oneself in the accompanied electronics equipment such as hardware, tablet computer, laptop.
Because of the presence of edge defect, in addition active force is weak between graphene layer, the graphene film that high temperature sintering is crossed is generally strong
Degree is all less high, is less than 100MPa, is unfavorable for its practical application.In addition, cross-linked structure and diamond lattic structure class between graphene layer
Seemingly, it is not damaged to thermally conductive, the heating conduction of graphene film will not be seriously affected.For this purpose, this patent exists two kinds of structure composites
Together, in the case where slight damage graphene film heating conduction, graphene film strength is improved.
Current graphene-based acoustic detector is based primarily upon single-layer graphene, but its absolute mechanics is lower, is easy breakage；
And micron thickness graphene thickness is too thick, it is insensitive to sound wave, and intensity is too low, is not suitable for acoustic detection；The graphene of nanometer thickness
The advantages of falling between, having both the two, but intensity is still insufficient.In addition, excessively high intensity can only detect high frequency sound wave,
Apparent response cannot be generated to low-frequency sound wave.It is necessary that the wave band for adapting to the frequency control of acoustic detection in human ear is wanted thus
Control film strength in a certain range.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of graphene film base low-frequency sound wave detector.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of graphene film base low-frequency sound wave detector is visited
It surveys device signal collection part to be made of graphene film and conductive substrates, the two is parallel, forms capacitance structure；Under sound wave effect,
Graphene film vibrates, and corresponding capacitance variations occur for acoustic detector；Graphene film with a thickness of 20-50nm, graphene
Interlayer crosslinking, the degree of cross linking are prepared in 1-5% by following steps：
(1) graphene oxide is configured to concentration less than 4mg/mL graphene oxide water solution, is slowly added to 10- inside
The fuming nitric aicd of 50% volume, 100-120 degrees Celsius of centrifuge washing after reflux 1-6 hours, obtains porous graphene oxide.It will
It is porous that graphene oxide is configured to concentration for 0.5-10ug/mL graphene oxide water solution, to filter 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, graphene film is supported in the conductive substrates by a nonconducting circular ring structure, circular ring structure
Height be not more than 10um.
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.
Currently, significant deficiency possessed by graphene film is intensity.The present invention utilizes the porous oxidation stone being etched
Black alkene film forming, and in the way of solid transfer, ultra-thin graphene film is obtained, is laid the foundation for the high resistance of device；Into one
Step increases graphene membrane surface fold by (1 DEG C/min) processing that slowly heats up, and extends the face of graphene film in unit space
Product；Then 2000 DEG C are set with 10 DEG C/min heating, to remove most atom defects inside graphene, but does not restore graphene
Internal stacked structure.Further by under ultra-thin graphene membrane surface splash-proofing sputtering metal particle, high temperature, metallic and graphene
Reaction forms metal carbides；Then metal carbides form metal chloride and loss under the action of chlorine, meanwhile, carbon
Structure changes to diamond lattic structure, greatly improves film strength 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 not will form AB packed structures.Carbon atom
Lacked in etching process, graphene because hole presence, carbon atom missing after, graphene because hole presence, modulus
It reduces, thus can realize low frequency under lesser intensity of sound or weaker sound wave by priming, so as to cause capacitance variations
Detection；Subsequent thin film is crosslinked between graphene layer after superchlorination, greatly increases the ultimate breaking strength of graphene film, so that
Film is easier to be resistant to high strong sound wave without being broken.
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 cross-linked graphene film and conductive substrates combine the capacitor model figure formed.Wherein, 1 is graphene film, 2
It is support for conductive substrates, 3.
Specific embodiment
Embodiment 1：
(1) 4mg/mL graphene oxide water solution is configured, the fuming nitric aicd of 10% volume is added, 100 degrees Celsius of reflux 6 are small
When after centrifuge washing, obtain porous graphene oxide.Its carbon content is measured compared to lacking 11.4% before etching.
It is 0.5ug/mL graphene oxide water solution that porous graphene oxide, which is configured to concentration, with hydrophilic polytetrafluoroethyl-ne
Alkene 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
Change the loss of titanium form.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 19nm.
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.After tested,
Graphene film intensity prepared by it is 8.4GPa.
As shown in figure 5, the circular ring structure (diameter 2cm, height 5um) that graphene film is made of by one polytetrafluoroethylene (PTFE)
It is supported in platinum substrate.Under certain frequency of sound wave and intensity, graphene film can shake, and cause capacitance variations, benefit
Capacitance size can be measured with LCR measuring appliance, to judge the frequency and intensity of sound wave.After tested, acoustic detector sound wave
Investigative range is 5-28KHZ, and sensitivity reaches 0.3HZ.
Embodiment 2：
(1) 2mg/mL graphene oxide water solution is configured, the fuming nitric aicd of 50% volume is slowly added to, 120 degrees Celsius are returned
Centrifuge washing after stream 1 hour, obtains porous graphene oxide.Its carbon content is measured compared to lacking before etching
36.8%.
(2) porous graphene oxide is configured to concentration is 10ug/mL graphene oxide water solution, using PC film as substrate
Filter film forming.
(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
Titanium 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 6.3GPa.
The circular ring structure (diameter 2cm, height 10um) that graphene film is made of by one polytetrafluoroethylene (PTFE) is supported in institute
It states in platinum substrate.Under certain frequency of sound wave and intensity, graphene film can shake, and cause capacitance variations, utilize LCR
Measuring appliance can measure capacitance size, to judge the frequency and intensity of sound wave.After tested, acoustic detector acoustic detection model
It encloses for 5-58KHZ, sensitivity reaches 0.3HZ.
Embodiment 3：
(1) 3mg/mL graphene oxide water solution is configured, is slowly added to the fuming nitric aicd of 20% volume inside, 100 take the photograph
Centrifuge washing after family name's degree flows back 5 hours, obtains porous graphene oxide.
(2) porous graphene oxide is configured to concentration is 1ug/mL graphene oxide water solution, using AAO film as substrate
Filter film forming.
(2) graphene oxide membrane for being attached at AAO film is placed in closed container, 90 degree of HI high temperature are up fumigated from bottom
0.5h。
(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
Change the loss of cobalt form.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 9.8GPa.
The circular ring structure (diameter 2cm, height 5um) that graphene film is made of by one polytetrafluoroethylene (PTFE) is supported in described
In platinum substrate.Under certain frequency of sound wave and intensity, graphene film can shake, and cause capacitance variations, be surveyed using LCR
Measuring device can measure capacitance size, to judge the frequency and intensity of sound wave.After tested, acoustic detector acoustic detection range
For 5-47KHZ, sensitivity reaches 0.3HZ.
Embodiment 4：
(1) 3mg/mL graphene oxide water solution is configured, is slowly added to the fuming nitric aicd of 20% volume inside, 100 take the photograph
Centrifuge washing after family name's degree flows back 5 hours, obtains porous graphene oxide.
(2) porous graphene oxide is configured to concentration is 3ug/mL graphene oxide water solution, using AAO film as substrate
Filter film forming.
(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
Change the loss of titanium form.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 9.1GPa.
The circular ring structure (diameter 2cm, height 5um) that graphene film is made of by one polytetrafluoroethylene (PTFE) is supported in described
In platinum substrate.Under certain frequency of sound wave and intensity, graphene film can shake, and cause capacitance variations, be surveyed using LCR
Measuring device can measure capacitance size, to judge the frequency and intensity of sound wave.After tested, after tested, acoustic detector sound wave
Investigative range is 5-37KHZ, and sensitivity reaches 0.3HZ.
Embodiment 5：
(1) 3mg/mL graphene oxide water solution is configured, is slowly added to the fuming nitric aicd of 20% volume inside, 100 take the photograph
Centrifuge washing after family name's degree flows back 5 hours, obtains porous graphene oxide.
(2) porous graphene oxide is configured to concentration is 10ug/mL graphene oxide water solution, using AAO film as base
Bottom filters film forming.
(2) graphene oxide membrane for being attached at AAO film is placed in closed container, 80 degree of HI high temperature are up fumigated from bottom
0.8h。
(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
Molybdenum 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 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
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 7.9GPa.
The circular ring structure (diameter 2cm, height 5um) that graphene film is made of by one polytetrafluoroethylene (PTFE) is supported in described
In platinum substrate.After tested, acoustic detector acoustic detection range is 4-22KHZ, and sensitivity reaches 0.3HZ.
Claims (5)
1. a kind of graphene film base low-frequency sound wave detector, which is characterized in that the detector signal collection part is by graphene
Film and conductive substrates are constituted, and the two is parallel, form capacitance structure；Under sound wave effect, graphene film vibrates, acoustic detection
Corresponding capacitance variations occur for device；The graphene film with a thickness of 20-50nm, be crosslinked between graphene layer, the degree of cross linking is in 1-
5%, graphene layer is interior to have nanoscale hole hole, is prepared by following steps：
(1) graphene oxide is configured to concentration less than 4mg/mL graphene oxide water solution, is added inside relative to oxidation
The fuming nitric aicd of graphene aqueous solution 10-50% volume, 100-120 degrees Celsius of centrifuge washing after reflux 1-6 hours, obtains porous
Graphene oxide.It is 0.5-10ug/mL graphene oxide water solution that porous graphene oxide, which is configured to concentration, to filter
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. high-strength graphite alkene film base acoustic detector according to claim 1, which is characterized in that the graphene film passes through
One nonconducting circular ring structure is supported in the conductive substrates, and the height of circular ring structure is not more than 10um.
3. the method as described in claim 1, which is characterized in that the solid transfer agent is selected from following substance, such as stone
Wax, naphthalene, arsenic trioxide, camphor, sulphur, norbornene, rosin etc. can distil or volatilize under certain conditions not soluble in water
Small molecule solid matter.
4. the method as described in claim 1, which is characterized in that the sublimation temperature of the solid transfer agent will be controlled 320
Below degree.
5. the method as described in claim 1, which is characterized in that the chlorination processing refers to：Sputtering there is into metal nanoparticle
Graphene film be placed in chlorine content be 0.5-10% environment in heated, time 0.1-4h.
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| CN108871547B (en) | 2021-01-01 |
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