CN105222920B - 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 PDF

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CN105222920B
CN105222920B CN201510645850.1A CN201510645850A CN105222920B CN 105222920 B CN105222920 B CN 105222920B CN 201510645850 A CN201510645850 A CN 201510645850A CN 105222920 B CN105222920 B CN 105222920B
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layer
graphene
temperature sensor
aluminum oxide
sensor
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CN201510645850.1A
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CN105222920A (en
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孙梦龙
吴云
霍帅
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中国电子科技集团公司第五十五研究所
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Abstract

The invention discloses a kind of CVD graphene temperature sensor, sensor-based system and temperature sensor preparation methods; temperature sensor therein is layer structure, from bottom to top successively includes rigid thermal conductive substrate layer, graphene layer, aluminum oxide buffer layer and aluminum oxide protective layer.Temperature sensor of the invention compared with prior art, the beneficial effect is that: 1) apparatus of the present invention structure simple, small in size, and thickness is thin, can bond body surface, easily operated.2) preparation method of apparatus of the present invention is simple, is not necessarily to power supply and lead, can avoid temperature drift.3) apparatus of the present invention total can keep stable structure at low temperatures and high temperatures, thus temperature measurement range is big, be suitable for a variety of environment.4) measurement method of apparatus of the present invention is contactless, and measuring targets influence is small, being capable of real-time monitoring.

Description

CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method

Technical field

The present invention relates to a kind of CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method, belong to half The technical field of conductor device.

Background technique

Graphene is by sp2The carbon atom of hydridization honeycomb crystal structure made of close-packed arrays in two-dimensional surface, only There is a carbon atom thickness, not only there are excellent photoelectric properties, also there is high mechanics and thermal property, thermal conductivity is high Up to 5300W/ (mK).Graphene can maintain self stability by forming fold on surface or adsorbing other molecules, and And it is able to bear biggish stress and strain, structural stability is still able to maintain under higher temperatures.

Raman spectrum analysis method is the scattering effect using light and a kind of non-destructive testing and characterization technique developed, graphene Raman spectrum be its molecular vibration and rotation embodiment.When graphene temperature changes, phonon structure can change Become, optical branch phonon LO (longitudinal direction) and TO (transverse direction) in plane, but the peak characteristic peak G of graphene is by this The optical branch sound of two long wavelengths is molecular, and therefore, the change of graphene temperature can make the peak its characteristic peak G shift.

Currently, temperature sensor in the market is broadly divided into four kinds: thermocouple, thermistor, resistance temperature detector (RTD) and IC temperature sensor.These four temperature sensors are required to external power supply and lead connection, and manufacture craft is multiple It is miscellaneous, for example, Chinese patent 201220337109.0, entitled " a kind of integral type thermocouple temperature sensor ";Utilize temperature-sensitive electricity The Chinese patent 201410042690.7 of temperature sensing is realized in resistance, entitled " a kind of temperature sensor production method ";It is Chinese special Benefit 201210438040.5, it is entitled " RTD system for detecting temperature ";Chinese patent 201280007908.4, entitled " semiconductor Temperature sensor " etc..

Compared with the method for sensing of the sensor, the present invention provides a kind of devices of contactless temperature sensing, and its Preparation method carries out temperature sensing using graphene characteristic peak position, and sensing device is connected without power supply with lead, preparation process Simply, temperature measurement range is big, is suitable for real-time measurement object or environment temperature, has huge application potential.

Summary of the invention

Goal of the invention: it is an object of the invention to propose a kind of CVD graphene temperature sensor, sensor-based system and temperature Transducer production method is based on graphite Raman Spectral Properties using the excellent heating conduction of semiconductor rigid substrate and graphene The corresponding relationship between peak G peak peak position and temperature is levied, realizes the non-contact real-time sensing to object or environment temperature, sensing device Without power supply and lead, preparation process is simple, and temperature measurement range is wide, is expected to become a kind of novel temperature sensing method.

Technical solution: temperature sensor of the present invention, the temperature sensor are layer structure, from bottom to top successively Including rigid thermal conductive substrate layer, graphene layer, aluminum oxide buffer layer and aluminum oxide protective layer.The temperature being thusly-formed The G summit of its Raman spectrum of sensor shifts with the temperature change of temperature sensor.

Further, the size of the graphene layer is less than the size of the rigid substrate layer, and the aluminum oxide is slow The size for rushing layer is greater than the size of graphene layer, and the aluminum oxide buffer layer covers the graphene layer, and described in cladding Graphene layer all around, so that graphene and ambient enviroment (such as gas, moisture) thoroughly separate, improves the anti-interference of sensor Performance.

Further, the graphene layer thickness single layer or 2-5 layers, for thickness in 0.3~2nm, the aluminum oxide is slow Rush layer with a thickness of 1~2nm, the aluminum oxide layer protective layer with a thickness of 10-50nm.

Further, the length of the rigid substrate layer is 5~30mm, and width is 5~30mm, the length of the graphene layer Degree is 5~20mm, and width is 5~20mm.

Further, including laser, incident optical, temperature sensor, the output optical fiber, spectroanalysis instrument and computer, The laser that laser issues is irradiated to the surface of temperature sensor, affiliated temperature sensor reflected laser signals by incident optical It is transmitted in spectroanalysis instrument by the output optical fiber, the data-signal of generation is sent in computer by spectroanalysis instrument.

The preparation method of temperature sensor of the invention, comprising the following steps:

1) it by 20~50 μm of 99% or more thickness of purity of copper foil, is dried after surface treatment;

2) graphene is grown on copper foil using chemical vapour deposition technique;

3) copper foil is transferred in rigid substrate;

4) one layer of Al is grown with low-power radio frequency sputtering method in the rigid substrate that transfer has graphene, is subsequently placed in air In make its autoxidation formed aluminum oxide buffer layer, lower sputtering power can ensure that graphene by it is lower damage and Reduce bonding probability;

5) one layer of aluminum oxide is grown with atomic layer deposition method on the aluminum oxide buffer layer that autoxidation is formed to protect Sheath is up to the temperature sensor.

Further, the step 2) grows graphene using chemical vapour deposition technique on copper foil, specifically:

H by copper foil at 950 DEG C~1030 DEG C230min is preheated in atmosphere, then passes to H2And CH4Mixed gas, H2Stream Amount is 40~80sccm, CH4Flow is 10~20sccm;After growing 10~30min at 950 DEG C~1030 DEG C, CH is closed4, H2Gas It is cooled to room temperature under atmosphere, single or double layer graphene is obtained on copper foil;

Further, copper foil is transferred in rigid substrate by the step 3), specifically:

There is the copper foil of graphene to cut growth, the PMMA of one layer of 500nm of spin coating dries 150s at 110 DEG C, it is placed in 0.5~ The FeCl of 1.0mol/L38~12h of aqueous solution soaking is cleaned 2~3 times in deionized water, is shifted later until copper foil is completely dissolved Among to preprepared rigid substrate, 90 DEG C of baking 2h are placed in acetone and dissolve PMMA, then ethyl alcohol, water cleaning, drying;

Further, the step 4) grows one layer of Al with radio frequency sputtering method in the rigid substrate that transfer has graphene, Being subsequently placed in air makes its autoxidation form aluminum oxide buffer layer, specifically:

Using radio frequency sputtering method transfer have graphene rigid substrate on grow one layer of very thin Al, sputtering power 2~ 20W, 60~180s of sputtering time, sputtering atmosphere Ar, 0.25~5.0Pa of air pressure;It is subsequently placed in air 1~2 day, makes it from oxygen Change, obtains the Al of 1~2nm2O3Buffer layer, to provide forming core while reducing damage of the graphene by dielectric growth technique Growth.

The step 5) grows one layer of three oxygen with atomic layer deposition method on the aluminum oxide buffer layer that autoxidation is formed Change two aluminium protective layers up to the temperature sensor, specifically:

One layer of 10~50nm Al is grown using atomic layer deposition method2O3Protective layer, the source Al used are trimethyl aluminium, this spirit 300mTorr is pressed, 150~250 DEG C of depositing temperature, deposits 100~500cyc of cycle.

Compared with prior art, the present invention the beneficial effect is that: 1) apparatus of the present invention structure is simple, small in size, and thickness is thin, Body surface can be bonded, it is easily operated.

2) preparation method of apparatus of the present invention is simple, is not necessarily to power supply and lead, can avoid temperature drift.

3) apparatus of the present invention total can keep stable structure, thus temperature measurement range at low temperatures and high temperatures Greatly, it is suitable for a variety of environment.

4) measurement method of apparatus of the present invention is contactless, and measuring targets influence is small, being capable of real-time monitoring.

Detailed description of the invention

Fig. 1 is the structural schematic diagram that the present invention carries out temperature sensing using graphene;

Fig. 2 is the preparation process schematic diagram of graphene sensing device;

Fig. 3 is the peak graphene G of the present invention peak position variation with temperature rule schematic diagram.

Specific embodiment

Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation Example.

Embodiment 1:

The present invention carries out the total schematic diagram of temperature sensing, such as Fig. 1 using temperature sensor 10 of the present invention It is shown, its working principles are as follows: laser 1 generates laser, temperature sensing device (dashed circle is irradiated to by incident optical 2 It is interior) graphene surface, sensing device and object under test 3 be in close contact, and reflected laser signals are transferred to light through the output optical fiber 11 In spectrum analysis instrument 4, the data of generation are transferred in computer 5 by spectroanalysis instrument 4, and computer carries out data processing, obtain object The temperature of body at this time realizes the real time temperature sensing of measuring targets.

The device of graphene temperature sensor is as shown in figure 1 shown in dashed circle and its enlarged drawing in the present invention, including thermally conductive The good rigid substrate 6 of property, is transferred to the graphene 7 in rigid substrate middle position, is covered in graphene and rigid substrate edge Al2O3The Al grown on buffer layer 8 and buffer layer2O3Protective layer 9.

The preparation process of graphene temperature sensing device is as shown in Fig. 2, firstly, in utilization chemical vapour deposition technique in copper foil Single or double layer graphene is grown on 10, is then spin coated onto one layer of PMMA film layer 11, then copper foil is dissolved, graphene is shifted It is one layer very thin in the growth of its surface using sputtering and autoxidation technology after dissolving PMMA to the good rigid basement 6 of thermal conductivity Al2O3Nucleation point finally grows one layer of Al using atomic layer deposition method2O3Protective layer.

Computer carries out the principle of data processing as shown in figure 3, position for the peak graphene characteristic peak G under different temperatures Difference takes T1To T2Several temperature in temperature range measure its corresponding peak G peak position, if obtain it is as shown in Figure 3 do, be based on These points carry out linear fit, can obtain linear relation ω (T)=ω between graphene G peak peak position and temperature0GT, At a temperature of middle ω (T) indicates T, the peak graphene G peak position, ω0The peak G peak position, χ when for zero degrees celsiusGIndicate the peak graphene G peak position Temperature drift rate.Based on this, the temperature of object under test is extrapolated by measuring the peak position graphene characteristic peak G.

The present invention provides a kind of preparation methods of the preparation method of CVD graphene temperature sensor, comprising the following steps:

1) prepare the copper foil for growing graphene, 20~50um of copper thickness, 99% or more purity is dried after surface treatment It is dry.

2) graphene is grown on copper foil using chemical vapor deposition (CVD) method.Its representative condition are as follows: by copper foil 950 ~1030 DEG C of H230min is preheated in atmosphere, then passes to H2And CH4Mixed gas, H2Flow is 40~80sccm, CH4Flow For 10~20sccm;After growing 10~30min at 950~1030 DEG C, CH is closed4, H2It is cooled to room temperature under atmosphere, on copper foil Obtain single or double layer graphene.

3) copper foil that growth has graphene is cut into required size, the PMMA of one layer of 500nm of spin coating dries at 110 DEG C 150s is placed in the FeCl of 0.5~1.0mol/L38~12h of aqueous solution soaking cleans 2 until copper foil is completely dissolved in deionized water ~3 times, among the good rigid substrate of the thermal conductivity being transferred to later, 90 DEG C of baking 2h are placed in acetone and dissolve PMMA, then second Alcohol, water cleaning, drying.

4) one layer of very thin Al, sputtering power 2 are grown in the rigid substrate that transfer has graphene using radio frequency sputtering method ~20W, 60~180s of sputtering time, sputtering atmosphere Ar, 0.25~5.0Pa of air pressure;It is subsequently placed in air 1~2 day, makes it certainly Oxidation, obtains the Al of 1~2nm2O3Buffer layer, so as to Al2O3The forming core of protective layer is grown.

5) one layer of 10~50nm Al is grown using atomic layer deposition (ALD) method2O3Protective layer, the source Al used are trimethyl Aluminium, background air pressure 300mTorr, 150~250 DEG C of depositing temperature, 100~500cyc of deposition cycle.

The present invention also provides a kind of test methods of graphene temperature sensing device: it is by sensing device and determinand Body is in close contact, and rigid substrate is thermally conductive rapidly, is consistent graphene temperature with object temperature;Swashed using what laser generated Light irradiates graphene, and laser is transmitted through optical fiber, and spectroanalysis instrument connect to receive reflection signal with computer, in real time Detect the Raman spectrum of graphene;When object temperature changes, the characteristic peak G summit of graphite Raman spectral line occurs inclined It moves, the temperature of object is extrapolated according to the peak characteristic peak G peak position.

Embodiment 1:

1) single or double layer graphene is grown on copper foil using chemical vapor deposition (CVD) method.It will be pure with a thickness of 30um Degree is dried after handling for 99% copper foil surface;It is subsequently placed in 1000 DEG C of H230min is preheated in atmosphere, is passed through H2And CH4Mixing Gas, H2Flow is 60sccm, CH4Flow is 15sccm;After growing 15min at 1000 DEG C, CH is closed4, H2It is cooled under atmosphere Room temperature obtains single or double layer graphene on copper foil.

2) it transfers graphene in SiC rigid substrate.There is the copper foil of graphene to be cut into 10mm growth in step 1) × 10mm size, the PMMA of one layer of 500nm of spin coating dry 150s at 110 DEG C, are placed in the FeCl of 1.0mol/L3Aqueous solution soaking 12h is cleaned 2~3 times in deionized water, is transferred in the SiC rigid substrate of 14mm × 14mm later until copper foil is completely dissolved Between, 90 DEG C of baking 2h are placed in acetone and dissolve PMMA, then ethyl alcohol, water cleaning, drying.

3)Al2O3The preparation of buffer layer.It is one layer very thin in the growth of step 2) resulting structures surface using radio frequency sputtering method Al, sputtering power 10W, sputtering time 60s, sputtering atmosphere Ar, air pressure 3.0Pa;It is subsequently placed in air 1~2 day, makes it from oxygen Change, obtains the Al of 1~2nm2O3Buffer layer, so as to Al2O3The forming core of protective layer is grown.

4)Al2O3The preparation of protective layer.One layer is grown in the structure that step 3) obtains using atomic layer deposition (ALD) method The Al of 20nm2O3Protective layer, the source Al used be trimethyl aluminium, background air pressure 300mTorr, 150 DEG C of depositing temperature, deposition cycle 200cyc。

5) graphene carries out the test method of temperature sensing device.Device obtained in step 4) and object under test is close Contact, SiC rigid substrate is thermally conductive rapidly, is consistent graphene temperature with object temperature;The laser generated using laser Graphene is irradiated, laser is transmitted through optical fiber, and spectroanalysis instrument connect to receive reflection signal with computer, is visited in real time The Raman spectrum of graphene is surveyed, is found when object temperature changes, the characteristic peak G summit of graphite Raman spectral line occurs inclined It moves as shown in Figure 3.It, can be according to the peak position at the peak characteristic peak G after the offset calibration of the peak characteristic peak G peak position at different temperatures Extrapolate the temperature of object.

As described above, must not be explained although the present invention has been indicated and described referring to specific preferred embodiment For the limitation to invention itself.It without prejudice to the spirit and scope of the invention as defined in the appended claims, can be right Various changes can be made in the form and details for it.

Claims (8)

1. a kind of sensor-based system based on CVD graphene temperature sensor, it is characterised in that: including laser (1), incident optical (2), CVD graphene temperature sensor (10), the output optical fiber (11), spectroanalysis instrument (4) and computer (5), laser (1) hair Laser out is irradiated to the surface of CVD graphene temperature sensor (10), the CVD graphene temperature by incident optical (2) Sensor (10) reflected laser signals are transmitted in spectroanalysis instrument (4) by the output optical fiber (11), and spectroanalysis instrument will generate Data-signal be sent in computer (5);
The CVD graphene temperature sensor is layer structure, from bottom to top successively includes rigid thermal conductive substrate layer (6), graphite Alkene layer (7), aluminum oxide buffer layer (8) and aluminum oxide protective layer (9).
2. the sensor-based system according to claim 1 based on CVD graphene temperature sensor, it is characterised in that: the stone The size of black alkene layer (7) is less than the size of the rigid thermal conductive substrate layer (6), the size of the aluminum oxide buffer layer (8) Greater than the size of graphene layer (7), the aluminum oxide buffer layer (8) covers the graphene layer (7), and coats the stone Black alkene layer (7) is all around.
3. the sensor-based system according to claim 1 or 2 based on CVD graphene temperature sensor, it is characterised in that: described Graphene layer (7) is single layer or 2-5 layers, with a thickness of 0.3~2nm, the aluminum oxide buffer layer (8) with a thickness of 1~ 3nm, the aluminum oxide protective layer (9) with a thickness of 5~50nm.
4. the sensor-based system according to claim 1 or 2 based on CVD graphene temperature sensor, it is characterised in that: described The length of rigid thermal conductive substrate layer (6) is 5~30mm, and width is 5~30mm, the length of the graphene layer (7) is 5~ 20mm, width are 5~20mm.
5. a kind of preparation method of CVD graphene temperature sensor, the CVD graphene temperature sensor is applied to claim In sensor-based system described in 1, it is characterised in that: the following steps are included:
(1) it by 20~50 μm of 99% or more thickness of purity of copper foil, is dried after hydrochloric acid solution immersion treatment;
(2) graphene is grown on copper foil using chemical vapour deposition technique;
(3) copper foil is transferred in rigid thermal conductive substrate;
(4) one layer of aluminium is grown with radio frequency sputtering method in the rigid thermal conductive substrate that transfer has graphene, being subsequently placed in air makes Its autoxidation forms aluminum oxide buffer layer;
(5) one layer of aluminum oxide protective layer is grown with atomic layer deposition method on the aluminum oxide buffer layer that autoxidation is formed Up to the CVD graphene temperature sensor.
6. the preparation method of CVD graphene temperature sensor according to claim 5, it is characterised in that: the step (2) Graphene is grown on copper foil using chemical vapour deposition technique, specifically: the H by copper foil at 950 DEG C~1030 DEG C2It is pre- in atmosphere Hot 30min then passes to H2 and CH4 mixed gas, H2Flow is 40~80sccm, CH4Flow is 10~20sccm;950 DEG C~ After growing 10~30min at 1030 DEG C, CH is closed4, H2It is cooled to room temperature under atmosphere, single or double layer graphite is obtained on copper foil Alkene.
7. the preparation method of CVD graphene temperature sensor according to claim 5, it is characterised in that: the step (3) Copper foil is transferred in rigid thermal conductive substrate, specifically: there is the copper foil of graphene to cut growth, one layer of PMMA of spin coating, thickness Range between 1~5000nm, baking temperature between 50~300 DEG C, baking time in 10~1000s, be placed in 0.01~ The FeCl of 1.0mol/L3Aqueous corrosion, 1~12h of etching time clean 1~10 until copper foil is completely dissolved in deionized water It is secondary, it is transferred among preprepared rigid thermal conductive substrate, after being dried 10~1000 minutes at 40~200 DEG C, is placed in later PMMA is dissolved in acetone, then ethyl alcohol, water cleaning, drying.
8. the preparation method of CVD graphene temperature sensor according to claim 5, it is characterised in that:
The step (4) grows one layer of aluminium with radio frequency sputtering method in the rigid thermal conductive substrate that transfer has graphene, is subsequently placed in Its autoxidation is set to form aluminum oxide buffer layer in air, specifically: there is the rigid of graphene in transfer using radio frequency sputtering method Property thermal conductive substrate on grow 1-2nm aluminium, 2~200W of sputtering power, 1~6000s of sputtering time, sputtering atmosphere should include Ar, N2、 He、H2, 0.25~5.0Pa of air pressure;It is subsequently placed in air 1~2 day, makes its autoxidation, obtain the aluminum oxide of 1~2nm Buffer layer, so that the forming core of aluminum oxide protective layer is grown;
The step (5) grows one layer of three oxidation two with atomic layer deposition method on the aluminum oxide buffer layer that autoxidation is formed Aluminium protective layer up to the CVD graphene temperature sensor, specifically: grow one layer of 10~50nm, tri- oxygen with atomic layer deposition method Change two aluminium protective layers, silicon source used is trimethyl aluminium, background air pressure 300mTorr, 50~250 DEG C of depositing temperature, deposition cycle 40 ~500 growth cycles.
CN201510645850.1A 2015-10-08 2015-10-08 CVD graphene temperature sensor, sensor-based system and temperature sensor preparation method CN105222920B (en)

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