CN105222920A - CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method - Google Patents
CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method Download PDFInfo
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- CN105222920A CN105222920A CN201510645850.1A CN201510645850A CN105222920A CN 105222920 A CN105222920 A CN 105222920A CN 201510645850 A CN201510645850 A CN 201510645850A CN 105222920 A CN105222920 A CN 105222920A
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Abstract
The invention discloses a kind of CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method; temperature sensor is wherein layer structure, comprises rigidity thermal conductive substrate layer, graphene layer, alundum (Al2O3) cushion and alundum (Al2O3) protective seam from bottom to top successively.Compared with prior art, its beneficial effect is temperature sensor of the present invention: 1) apparatus of the present invention structure is simple, and volume is little, and thickness is thin, can dung surface, is easy to operation.2) preparation method of apparatus of the present invention is simple, without the need to power supply and lead-in wire, can avoid temperature drift.3) apparatus of the present invention total all can be stablized by holding structure at low temperatures and high temperatures, and thus temperature measurement range is large, is applicable to multiple environment.4) measuring method of apparatus of the present invention is contactless, and measuring targets impact is little, can Real-Time Monitoring.
Description
Technical field
The present invention relates to a kind of CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method, belong to the technical field of semiconductor devices.
Background technology
Graphene is by sp
2the cellular crystal structure of carbon atom close-packed arrays in two dimensional surface of hydridization, only has a carbon atom thickness, and not only have excellent photoelectric properties, also have high mechanics and thermal property, its thermal conductivity is up to 5300W/ (mK).Graphene can maintain self stability by forming fold on surface or adsorbing other molecules, and can bear larger stress and strain, still can holding structure stability under higher temperatures.
Raman spectrum analysis method utilizes the scattering effect of light and a kind of Non-Destructive Testing of developing and characterization technique, and the Raman spectrum of Graphene is the embodiment of its molecular vibration and rotation.When Graphene temperature changes, its phonon structure can change, particularly be positioned at optical branch phonon LO (longitudinal direction) and the TO (transverse direction) of plane, but the characteristic peak G peak of Graphene is molecular by the optical branch sound of these two long wavelengths, therefore, the change of Graphene temperature can make its characteristic peak G peak offset.
At present, the temperature sensor on market is mainly divided into four kinds: thermopair, thermistor, resistance temperature detector (RTD) and IC temperature sensor.These four kinds of temperature sensors all need external power source, and lead-in wire connects, and complex manufacturing technology, such as, Chinese patent 201220337109.0, name is called " a kind of integral type thermocouple temperature sensor "; Utilize thermistor to realize the Chinese patent 201410042690.7 of temperature sensing, name is called " a kind of temperature sensor production method "; Chinese patent 201210438040.5, name is called " RTD system for detecting temperature "; Chinese patent 201280007908.4, name is called " semiconductor temperature sensor ".
Compared with the method for sensing of the sensor, the invention provides a kind of device of contactless temperature sensing, and preparation method thereof, Graphene characteristic peak position is utilized to carry out temperature sensing, sensing device is connected with lead-in wire without the need to power supply, and preparation technology is simple, and temperature measurement range is large, be applicable to measure object or environment temperature in real time, there is huge application potential.
Summary of the invention
Goal of the invention: the object of the invention is to propose a kind of CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method, utilize semiconductor rigid substrate and the excellent heat conductivility of Graphene, based on the corresponding relation between G peak-to-peak position, graphite Raman spectral signature peak and temperature, realize the noncontact real-time sensing to object or environment temperature, sensing device is without the need to power supply and lead-in wire, preparation technology is simple, and temperature measurement range is wide, is expected to become a kind of novel temperature sensing method.
Technical scheme: temperature sensor of the present invention, described temperature sensor is layer structure, comprises rigidity thermal conductive substrate layer, graphene layer, alundum (Al2O3) cushion and alundum (Al2O3) protective seam from bottom to top successively.The G summit of its Raman spectrum of temperature sensor of formation like this offsets along with the temperature variation of temperature sensor.
Further, the size of described graphene layer is less than the size of described rigid substrate layer, the size of described alundum (Al2O3) cushion is greater than the size of graphene layer, described alundum (Al2O3) cushion covers described graphene layer, and coated described graphene layer all around, so that Graphene and surrounding environment (as gas, moisture etc.) thoroughly separate, improve the interference free performance of sensor.
Further, described graphene layer thickness individual layer or 2-5 layer, thickness is at 0.3 ~ 2nm, and the thickness of described alundum (Al2O3) cushion is 1 ~ 2nm, and the thickness of described alundum (Al2O3) layer protective seam is 10-50nm.
Further, the length of described rigid substrate layer is 5 ~ 30mm, and width is 5 ~ 30mm, and the length of described graphene layer is 5 ~ 20mm, and width is 5 ~ 20mm.
Further, comprise laser instrument, incident optical, temperature sensor, outgoing optical fiber, spectroanalysis instrument and computing machine, the laser that laser instrument sends is irradiated to the surface of temperature sensor through incident optical, affiliated temperature sensor reflected laser signals transfers in spectroanalysis instrument through outgoing optical fiber, and the data-signal of generation is sent in computing machine by spectroanalysis instrument.
The preparation method of temperature sensor of the present invention, comprises the following steps:
1) by the Copper Foil of purity more than 99% thickness 20 ~ 50 μm, surface treatment post-drying;
2) chemical vapour deposition technique growing graphene on Copper Foil is utilized;
3) Copper Foil is transferred in rigid substrate;
4) have in the rigid substrate of Graphene and grow one deck Al in transfer with low-power radio frequency sputtering method, then being placed in air makes its autoxidation form alundum (Al2O3) cushion, and lower sputtering power can guarantee that Graphene is subject to lower damage and is reduced to key probability;
5) on the alundum (Al2O3) cushion of autoxidation formation, grow one deck alundum (Al2O3) protective seam with atomic layer deposition method and namely obtain described temperature sensor.
Further, described step 2) utilize chemical vapour deposition technique growing graphene on Copper Foil, be specially:
By the H of Copper Foil at 950 DEG C ~ 1030 DEG C
2in atmosphere, preheating 30min, then passes into H
2and CH
4mixed gas, H
2flow is 40 ~ 80sccm, CH
4flow is 10 ~ 20sccm; After growing 10 ~ 30min at 950 DEG C ~ 1030 DEG C, close CH
4, H
2be cooled to room temperature under atmosphere, Copper Foil obtains individual layer or bilayer graphene;
Further, described step 3) Copper Foil is transferred in rigid substrate, be specially:
Growth is had the Copper Foil cutting of Graphene, the PMMA of spin coating one deck 500nm, dries 150s at 110 DEG C, is placed in the FeCl of 0.5 ~ 1.0mol/L
3aqueous solution soaking 8 ~ 12h, dissolves completely to Copper Foil, cleans 2 ~ 3 times, be transferred in the middle of preprepared rigid substrate afterwards in deionized water, and 90 DEG C are dried 2h, are placed in acetone and dissolve PMMA, and then ethanol, water cleaning, dry;
Further, described step 4) to have in the rigid substrate of Graphene in transfer and grow one deck Al with radio frequency sputtering method, be then placed in air and make its autoxidation form alundum (Al2O3) cushion, be specially:
Utilize radio frequency sputtering method to have in the rigid substrate of Graphene in transfer and grow the very thin Al of one deck, sputtering power 2 ~ 20W, sputtering time 60 ~ 180s, sputtering atmosphere Ar, air pressure 0.25 ~ 5.0Pa; Then be placed in air 1 ~ 2 day, make its autoxidation, obtain the Al of 1 ~ 2nm
2o
3cushion, to provide forming core to grow while reducing the damage of Graphene by dielectric growth technique.
Described step 5) the alundum (Al2O3) cushion that formed in autoxidation grows one deck alundum (Al2O3) protective seam with atomic layer deposition method and namely obtains described temperature sensor, be specially:
Atomic layer deposition method is utilized to grow one deck 10 ~ 50nmAl
2o
3protective seam, Al source used is trimethyl aluminium, background air pressure 300mTorr, depositing temperature 150 ~ 250 DEG C, deposition cycle 100 ~ 500cyc.
Compared with prior art, its beneficial effect is in the present invention: 1) apparatus of the present invention structure is simple, and volume is little, and thickness is thin, can dung surface, is easy to operation.
2) preparation method of apparatus of the present invention is simple, without the need to power supply and lead-in wire, can avoid temperature drift.
3) apparatus of the present invention total all can be stablized by holding structure at low temperatures and high temperatures, and thus temperature measurement range is large, is applicable to multiple environment.
4) measuring method of apparatus of the present invention is contactless, and measuring targets impact is little, can Real-Time Monitoring.
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes Graphene to carry out the structural representation of temperature sensing;
Fig. 2 is the preparation process schematic diagram of Graphene sensing device;
Fig. 3 is Graphene G peak-to-peak position of the present invention variation with temperature rule schematic diagram.
Embodiment
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
The present invention utilizes temperature sensor 10 of the present invention to carry out the total schematic diagram of temperature sensing, as shown in Figure 1, its principle of work is as follows: laser instrument 1 produces laser, the graphenic surface of temperature sensing device (in dashed circle) is irradiated to by incident optical 2, sensing device and object under test 3 close contact, reflected laser signals is transferred in spectroanalysis instrument 4 through outgoing optical fiber 11, the data of generation are transferred in computing machine 5 by spectroanalysis instrument 4, computing machine carries out data processing, draw object temperature now, realize the real time temperature sensing of measuring targets.
In the present invention, the device of graphene temperature sensor is as shown in dashed circle in Fig. 1 and enlarged drawing thereof, comprises the good rigid substrate of thermal conductivity 6, is transferred to the Graphene 7 in rigid substrate centre position, is covered in the Al at Graphene and rigid substrate edge
2o
3cushion 8, and the Al that cushion grows
2o
3protective seam 9.
The preparation process of Graphene temperature sensing device as shown in Figure 2, first, on Copper Foil 10, individual layer or bilayer graphene is grown utilizing chemical vapour deposition technique, then spin coating one deck PMMA thin layer 11, then Copper Foil is dissolved, Graphene is transferred in the good stiff base of thermal conductivity 6, dissolves after PMMA, utilize sputtering and autoxidation technology at the very thin Al of its superficial growth one deck
2o
3forming core point, finally utilizes atomic layer deposition method to grow one deck Al
2o
3protective seam.
Computing machine carries out the principle of data processing as shown in Figure 3, and the position for Graphene characteristic peak G peak under different temperatures is different, gets T
1to T
2some temperature in temperature range, measure the G peak-to-peak position of its correspondence, obtain some points as shown in Figure 3, carry out linear fit, can draw linear relation ω (the T)=ω between Graphene G peak-to-peak position and temperature based on these points
0+ χ
gt, under wherein ω (T) represents T temperature, Graphene G peak-to-peak position, ω
0for G peak-to-peak position during zero degrees celsius, χ
grepresent the temperature drift rate of Graphene G peak-to-peak position.Based on this, extrapolate the temperature of object under test by measuring Graphene characteristic peak G peak position.
The invention provides the preparation method of a kind of preparation method of CVD graphene temperature sensor, comprise the following steps:
1) Copper Foil being used for growing graphene is prepared, copper thickness 20 ~ 50um, purity more than 99%, surface treatment post-drying.
2) chemical vapor deposition (CVD) method growing graphene on Copper Foil is utilized.Its representative condition is: by the H of Copper Foil at 950 ~ 1030 DEG C
2in atmosphere, preheating 30min, then passes into H
2and CH
4mixed gas, H
2flow is 40 ~ 80sccm, CH
4flow is 10 ~ 20sccm; After growing 10 ~ 30min at 950 ~ 1030 DEG C, close CH
4, H
2be cooled to room temperature under atmosphere, Copper Foil obtains individual layer or bilayer graphene.
3) have the Copper Foil of Graphene to be cut into required size growth, the PMMA of spin coating one deck 500nm, dries 150s at 110 DEG C, is placed in the FeCl of 0.5 ~ 1.0mol/L
3aqueous solution soaking 8 ~ 12h, dissolves completely to Copper Foil, cleans 2 ~ 3 times in deionized water, and in the middle of the rigid substrate that the thermal conductivity be transferred to afterwards is good, 90 DEG C are dried 2h, are placed in acetone and dissolve PMMA, and then ethanol, water cleaning, dry.
4) utilize radio frequency sputtering method to have in the rigid substrate of Graphene in transfer and grow the very thin Al of one deck, sputtering power 2 ~ 20W, sputtering time 60 ~ 180s, sputtering atmosphere Ar, air pressure 0.25 ~ 5.0Pa; Then be placed in air 1 ~ 2 day, make its autoxidation, obtain the Al of 1 ~ 2nm
2o
3cushion, so that Al
2o
3the forming core growth of protective seam.
5) ald (ALD) method is utilized to grow one deck 10 ~ 50nmAl
2o
3protective seam, Al source used is trimethyl aluminium, background air pressure 300mTorr, depositing temperature 150 ~ 250 DEG C, deposition cycle 100 ~ 500cyc.
Present invention also offers a kind of method of testing of Graphene temperature sensing device: it is by sensing device and object under test close contact, the rapid heat conduction of rigid substrate makes Graphene temperature and object temperature be consistent; The laser utilizing laser instrument to produce irradiates Graphene, and laser transmits through optical fiber, and spectroanalysis instrument receives reflected signal, and is connected with computing machine, the Raman spectrum of real-time detection Graphene; When object temperature changes, the characteristic peak G summit of graphite Raman spectral line offsets, and extrapolates the temperature of object according to characteristic peak G peak-to-peak position.
Embodiment 1:
1) utilize chemical vapor deposition (CVD) method on Copper Foil, grow individual layer or bilayer graphene.Be 30um by thickness, purity is the copper foil surface process post-drying of 99%; Then the H of 1000 DEG C is placed in
2in atmosphere, preheating 30min, passes into H
2and CH
4mixed gas, H
2flow is 60sccm, CH
4flow is 15sccm; After growing 15min at 1000 DEG C, close CH
4, H
2be cooled to room temperature under atmosphere, Copper Foil obtains individual layer or bilayer graphene.
2) Graphene is transferred in SiC rigid substrate.By step 1) in growth have the Copper Foil of Graphene to be cut into 10mm × 10mm size, the PMMA of spin coating one deck 500nm, dries 150s at 110 DEG C, is placed in the FeCl of 1.0mol/L
3aqueous solution soaking 12h, dissolves completely to Copper Foil, cleans 2 ~ 3 times in deionized water, and in the middle of the SiC rigid substrate being transferred to 14mm × 14mm afterwards, 90 DEG C are dried 2h, are placed in acetone and dissolve PMMA, and then ethanol, water cleaning, dry.
3) Al
2o
3the preparation of cushion.Utilize radio frequency sputtering method in step 2) Al that resulting structures superficial growth one deck is very thin, sputtering power 10W, sputtering time 60s, sputtering atmosphere Ar, air pressure 3.0Pa; Then be placed in air 1 ~ 2 day, make its autoxidation, obtain the Al of 1 ~ 2nm
2o
3cushion, so that Al
2o
3the forming core growth of protective seam.
4) Al
2o
3the preparation of protective seam.Utilize ald (ALD) method in step 3) structure that obtains grows the Al of one deck 20nm
2o
3protective seam, Al source used is trimethyl aluminium, background air pressure 300mTorr, depositing temperature 150 DEG C, deposition cycle 200cyc.
5) Graphene carries out the method for testing of temperature sensing device.By step 4) in the device that obtains and object under test close contact, the rapid heat conduction of SiC rigid substrate, makes Graphene temperature and object temperature be consistent; The laser utilizing laser instrument to produce irradiates Graphene, laser transmits through optical fiber, spectroanalysis instrument receives reflected signal, and be connected with computing machine, the Raman spectrum of real-time detection Graphene, finding when object temperature changes, there is skew as shown in Figure 3 in the characteristic peak G summit of graphite Raman spectral line.After demarcating according to the skew at different temperatures of characteristic peak G peak-to-peak position, the temperature of object can be extrapolated according to the peak position at characteristic peak G peak.
As mentioned above, although represented with reference to specific preferred embodiment and described the present invention, it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention prerequisite not departing from claims definition, various change can be made in the form and details to it.
Claims (9)
1. a CVD graphene temperature sensor; it is characterized in that; described temperature sensor is layer structure, comprises rigidity thermal conductive substrate layer (6), graphene layer (7), alundum (Al2O3) cushion (8) and alundum (Al2O3) protective seam (9) from bottom to top successively.
2. CVD graphene temperature sensor according to claim 1, it is characterized in that, the size of described graphene layer (7) is less than the size of described rigid substrate layer (6), the size of described alundum (Al2O3) cushion (8) is greater than the size of graphene layer (7), described alundum (Al2O3) cushion (8) covers described graphene layer (7), and coated described graphene layer (7) all around.
3. CVD graphene temperature sensor according to claim 1 and 2; it is characterized in that; described graphene layer (7) individual layer or 2-5 layer; thickness is 0.3 ~ 2nm; the thickness of described alundum (Al2O3) cushion (8) is 1 ~ 3nm, and the thickness of described alundum (Al2O3) layer protective seam (9) is 5 ~ 50nm.
4. CVD graphene temperature sensor according to claim 1 and 2, it is characterized in that, the length of described rigid substrate layer (6) is 5 ~ 30mm, and width is 5 ~ 30mm, the length of described graphene layer (7) is 5 ~ 20mm, and width is 5 ~ 20mm.
5. comprise the sensor-based system of the arbitrary described CVD graphene temperature sensor of Claims 1 to 4, it is characterized in that, comprise laser instrument (1), incident optical (2), temperature sensor (10), outgoing optical fiber (11), spectroanalysis instrument (4) and computing machine (5), the laser that laser instrument (1) sends is irradiated to the surface of temperature sensor (10) through incident optical (2), affiliated temperature sensor (10) reflected laser signals transfers in spectroanalysis instrument (4) through outgoing optical fiber (11), the data-signal of generation is sent in computing machine (5) by spectroanalysis instrument.
6. a CVD graphene temperature sensor preparation method, is characterized in that, comprises the following steps:
1) by the Copper Foil of purity more than 99% thickness 20 ~ 50 μm, through hydrochloric acid solution immersion treatment post-drying;
2) chemical vapour deposition technique growing graphene on Copper Foil is utilized;
3) Copper Foil is transferred in rigid substrate;
4) have in the rigid substrate of Graphene and grow one deck Al in transfer with radio frequency sputtering method, be then placed in air and make its autoxidation form alundum (Al2O3) cushion;
5) on the alundum (Al2O3) cushion of autoxidation formation, grow one deck alundum (Al2O3) protective seam with atomic layer deposition method and namely obtain described temperature sensor.
7. temperature sensor preparation method according to claim 6, is characterized in that, described step 2) utilize chemical vapour deposition technique growing graphene on Copper Foil, be specially:
By the H of Copper Foil at 950 DEG C ~ 1030 DEG C
2preheating 30min in atmosphere, then passes into H2 and CH4 mixed gas, H
2flow is 40 ~ 80sccm, CH
4flow is 10 ~ 20sccm; After growing 10 ~ 30min at 950 DEG C ~ 1030 DEG C, close CH
4, H
2be cooled to room temperature under atmosphere, Copper Foil obtains individual layer or bilayer graphene.
8. temperature sensor preparation method according to claim 6, is characterized in that,
Described step 3) Copper Foil is transferred in rigid substrate, be specially:
Growth is had the Copper Foil cutting of Graphene, spin coating one deck PMMA, thickness range is between 1 ~ 5000nm, and baking temperature is between 50 ~ 300 DEG C, and baking time, at 10 ~ 1000s, is placed in the FeCl of 0.01 ~ 1.0mol/L
3aqueous corrosion, etching time 1 ~ 12h, dissolves completely to Copper Foil, clean 1 ~ 10 time in deionized water, be transferred in the middle of preprepared rigid substrate afterwards, dry after 10 ~ 1000 minutes at 40 ~ 200 DEG C, be placed in acetone and dissolve PMMA, then ethanol, water cleaning, dry.
9. temperature sensor preparation method according to claim 6, is characterized in that,
Described step 4) have in the rigid substrate of Graphene and grow one deck Al in transfer with radio frequency sputtering method, be then placed in air and make its autoxidation form alundum (Al2O3) cushion, be specially:
Utilize radio frequency sputtering method to have in the rigid substrate of Graphene in transfer and grow 1-2nmAl, sputtering power 2 ~ 200W, sputtering time 1 ~ 6000s, sputtering atmosphere should comprise Ar, N
2, He, H
2, air pressure 0.25 ~ 5.0Pa; Then be placed in air 1 ~ 2 day, make its autoxidation, obtain the Al of 1 ~ 2nm
2o
3cushion, so that Al
2o
3the forming core growth of protective seam;
Described step 5) the alundum (Al2O3) cushion that formed in autoxidation grows one deck alundum (Al2O3) protective seam with atomic layer deposition method and namely obtains described temperature sensor, be specially:
Ald (ALD) method is utilized to grow one deck 10 ~ 50nmAl
2o
3protective seam, Al source used is trimethyl aluminium, background air pressure 300mTorr, depositing temperature 50 ~ 250 DEG C, deposition cycle 40 ~ 500 growth cycles.
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|---|---|
| CN105222920B (en) | 2019-01-25 |
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