CN104359561B - A kind of flexible infrared sensor based on carbon nano pipe array and preparation method thereof - Google Patents
A kind of flexible infrared sensor based on carbon nano pipe array and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of flexible infrared sensor based on carbon nano pipe array and preparation method thereof, belong to flexible infrared sensor preparation field.Including substrate and positioned at the infrared-sensitive material of substrate, the infrared-sensitive material is to be provided with electrode on p-type carbon nano pipe array and the P N knots of n type carbon nanotube array formation, the p-type carbon nano pipe array and n type carbon nanotube array.The P N knots that the flexible infrared sensor is constituted using p-type carbon nano pipe array and n type carbon nanotube array are used as infrared-sensitive material, when device is by Infrared irradiation, infrared response can be characterized by testing P N knot open-circuit voltages, reduce power consumption, without using voltage or current source table, convenient use, and the repeatable bending of the flexible sensor is without influenceing the performance of device, with good stability.
Description
Technical field
The invention belongs to carbon nanomaterial synthesis and flexible infrared sensor preparation field, and in particular to one kind is received based on carbon
Flexible infrared sensor of mitron array and preparation method thereof.
Background technology
Infrared sensor be widely used in Woundless blood sugar monitoring, rhythm of the heart, Intelligent housing and it is infrared into
The fields such as picture.At present, with it is more and more wearable or can winding apparatus widely use, for the need of flexible sensor
Ask more and more urgent, the research to flexible sensor is also increasingly paid attention to by researcher.With traditional infrared sensor phase
Than flexible infrared sensor not only needs infrared-sensitive material to have good infrared response, it is often more important that needs are applied to
The material of flexible infrared sensor remains in that good performance in the state of bending.
CNT is that (radial dimension is nanometer scale to a kind of special construction, and axial dimension is micron dimension, pipe two ends
Substantially all seal) One-dimensional Quantum material, there is excellent mechanics, electricity, chemistry and mechanical performance, lightweight, by
People have been arrived greatly to pay close attention to.In recent years, deepening continuously with CNT and nano materials research, before its wide application
Scape is constantly displayed.Because the characteristic electron of CNT is mainly the structures shape by its atomic arrangement, so its stress
Change or the change of chemisorbed can all produce influence to electrical conductivity, its changing value can detect by current signal, these properties
So that CNT can be used as sensor.Change the diameter and dopant states of CNT simultaneously, its band gap can be adjusted several
Change in hundreds of meV, and the energy range of infrared light (1~15 μm) wave band is 1.24eV~83meV, the taboo with CNT
Bandwidth is close, therefore in theory, CNT can be used as infrared sensor.At present, using CNT or carbon
Nanometer tube composite materials prepare infrared sensor as sensitive material, still, because the sensor is by testing CNT
The change of resistance under infrared radiation, therefore need to measure in CNT two ends applied voltage or current source.
The content of the invention
A kind of defect that the present invention exists for background technology, it is proposed that flexible infrared sensing based on carbon nano pipe array
Device and preparation method thereof.The P-N that the flexible infrared sensor is constituted using p-type carbon nano pipe array and n type carbon nanotube array
Knot, when device is by Infrared irradiation, can characterize infrared sound as infrared-sensitive material by testing P-N junction open-circuit voltage
Should, power consumption is reduced, without using voltage or current source table, the repeatable bending of convenient use, and the flexible sensor is without shadow
The performance of Chinese percussion instrument part, with good stability.
Technical scheme is as follows：
A kind of flexible infrared sensor based on carbon nano pipe array, including substrate and the infrared-sensitive positioned at substrate
Material, the infrared-sensitive material is the P-N junction of p-type carbon nano pipe array and the formation of n type carbon nanotube array, the p-type carbon
Electrode is provided with nano-tube array and n type carbon nanotube array.
Further, the substrate is polymethyl methacrylate (PMMA), the p-type carbon nano pipe array and N-type carbon
The electrode set on nano-tube array is silver electrode, is obtained by conductive silver paste solidification.
The preparation method of the above-mentioned flexible infrared sensor based on carbon nano pipe array, comprises the following steps：
Step 1：Prepare methyl phenyl ethers anisole solution of the mass concentration for 0.08g/mL polymethyl methacrylate；
Step 2：P-type carbon nano pipe array and n type carbon nanotube are prepared using floating catalytic chemical vapour deposition technique respectively
Array；
Step 3：The polymethylacrylic acid that step 1 is prepared is dripped on the substrate with p-type carbon nano pipe array that step 2 is obtained
The methyl phenyl ethers anisole solution of methyl esters to whole covering substrates stop, and are put into baking oven and dry, after after polymethyl methacrylate solidification, by it
Peeled off from substrate, obtain the polymethyl methacrylate with p-type carbon nano pipe array, then will be with p-type carbon nano pipe array
Polymethyl methacrylate be fitted tightly on the substrate with n type carbon nanotube array that step 2 is obtained to ensure that p-type carbon is received
Seamless between mitron array and n type carbon nanotube array, the methyl phenyl ethers anisole solution for the polymethyl methacrylate that drop step 1 is prepared is extremely
Whole covering substrates stop, and are put into baking oven and dry, and after after polymethyl methacrylate solidification, it is peeled off from substrate, that is, existed
The p-type carbon nano pipe array and n type carbon nanotube array being laminated on polymethyl methacrylate；
Step 4：Electrode is prepared on the p-type carbon nano pipe array and n type carbon nanotube array obtained in step 3.
Further, it is by temperature when dripping the methyl phenyl ethers anisole solution drying for having polymethyl methacrylate described in step 3
150 DEG C, drying time is 20min；The electricity prepared described in step 4 on p-type carbon nano pipe array and n type carbon nanotube array
Extremely silver electrode, is obtained by conductive silver paste solidification.
The preparation method of the above-mentioned flexible infrared sensor based on carbon nano pipe array, comprises the following steps：
Step 1：Prepare methyl phenyl ethers anisole solution of the mass concentration for 0.08g/mL polymethyl methacrylate；
Step 2：P-type carbon nano pipe array and n type carbon nanotube are prepared using floating catalytic chemical vapour deposition technique respectively
Array；
Step 3：The polymethylacrylic acid that step 1 is prepared is dripped on the substrate with n type carbon nanotube array that step 2 is obtained
The methyl phenyl ethers anisole solution of methyl esters to whole covering substrates stop, and are put into baking oven and dry, after after polymethyl methacrylate solidification, by it
Peeled off from substrate, obtain the polymethyl methacrylate with n type carbon nanotube array, then will be with n type carbon nanotube array
Polymethyl methacrylate be fitted tightly on the substrate with p-type carbon nano pipe array that step 2 is obtained to ensure that N-type carbon is received
Seamless between mitron array and p-type carbon nano pipe array, the methyl phenyl ethers anisole solution for the polymethyl methacrylate that drop step 1 is prepared is extremely
Whole covering substrates stop, and are put into baking oven and dry, and after after polymethyl methacrylate solidification, it is peeled off from substrate, that is, existed
The n type carbon nanotube array and p-type carbon nano pipe array being laminated on polymethyl methacrylate；
Step 4：Electrode is prepared on the n type carbon nanotube array and p-type carbon nano pipe array obtained in step 3.
Further, it is by temperature when dripping the methyl phenyl ethers anisole solution drying for having polymethyl methacrylate described in step 3
150 DEG C, drying time is 20min；The electricity prepared described in step 4 on n type carbon nanotube array and p-type carbon nano pipe array
Extremely silver electrode, is obtained by conductive silver paste solidification.
Further, the preparation process of p-type carbon nano pipe array described in step 2 is：Using ferrocene as solute, toluene is
Solvent, the toluene solution for preparing mass fraction for 3% ferrocene is used as precursor liquid；Silicon dioxide substrates are placed in tube furnace
It is interior, tubular type in-furnace temperature is heated to 850 DEG C under an argon atmosphere, the forerunner of above-mentioned preparation is then injected with 10mL/h speed
Liquid, is heat-treated 30min under 850 DEG C, the mixed-gas atmosphere of argon gas and hydrogen, makes CNT raw in silicon dioxide substrates
It is long；After heat treatment terminates, room temperature is naturally cooled to stove under an argon atmosphere, i.e., p-type carbon is obtained in silicon dioxide substrates and is received
Mitron array.
Further, in the mixed gas of above-mentioned argon gas and hydrogen, the percent by volume of argon gas is 94%, the volume of hydrogen
Percentage is 6%.
Further, the preparation process of n type carbon nanotube array described in step 2 is：Using ferrocene as solute, acetonitrile and
Alcohol mixed solution is solvent, prepare mass fraction for 2% solution of ferrocene as precursor liquid, wherein acetonitrile and ethanol matter
Amount is than being 16:1；Silicon dioxide substrates are placed in tube furnace, tubular type in-furnace temperature is heated to 850 DEG C under an argon atmosphere,
Then the precursor liquid of above-mentioned preparation is injected with 8mL/h speed, under 850 DEG C, the mixed-gas atmosphere of argon gas and hydrogen at heat
30min is managed, CNT is grown in silicon dioxide substrates；After heat treatment terminates, under an argon atmosphere with stove natural cooling
To room temperature, i.e., n type carbon nanotube array is obtained in silicon dioxide substrates.
Further, in the mixed gas of above-mentioned argon gas and hydrogen, the percent by volume of argon gas is 94%, the volume of hydrogen
Percentage is 6%.
Beneficial effects of the present invention are：
1st, the sensitive material for the flexible infrared sensor that the present invention is provided is p-type carbon nano pipe array and n type carbon nanotube
There is N to point to P built in field between the P-N junction of array composition, P-N junction, when the flexible infrared sensor is by infrared radiation,
The unnecessary carrier produced can be moved in the presence of built in field, and wherein electronics flows to N sides, and hole flows to P sides, from
And the change of phase boundary potential is there occurs on P-N junction surface, it is outside then can pass through p-type carbon nano pipe array and n type carbon nanotube battle array
Silver electrode on row detects voltage.
2nd, the flexible infrared sensor power consumption that the present invention is provided is extremely low, it is not necessary to voltage or current source table, convenient application；Adopt
Infrared-sensitive material carbon nano-pipe array will not be damaged when being listed in substrate bending, make the repeatable bending of sensor without influenceing device
The performance of part, with good stability；Flexible infrared sensor that the present invention is provided prepares that cost is low, technique is simple, is applicable
In progress industrial production.
Brief description of the drawings
Fig. 1 is the structural representation for the flexible infrared sensor based on carbon nano pipe array that the embodiment of the present invention is obtained.
Fig. 2 is the scanning electron microscope diagram (SEM) for the carbon nano pipe array that the embodiment of the present invention is prepared.Wherein,
(a) it is the scanning electron microscope (SEM) photograph of p-type carbon nano pipe array, (b) is the scanning electron microscope (SEM) photograph of n type carbon nanotube array.
Fig. 3 is the x-ray photoelectron energy spectrum diagram (XPS) for the n type carbon nanotube array that the embodiment of the present invention is obtained.
Fig. 4 is the obtained flexible infrared sensor based on carbon nano pipe array of the embodiment of the present invention in 850nm wavelength
Response curve.
Embodiment
The present invention is described further with reference to the accompanying drawings and examples.
A kind of flexible infrared sensor based on carbon nano pipe array, including substrate and the infrared-sensitive positioned at substrate
Material, the infrared-sensitive material is the P-N junction of p-type carbon nano pipe array and the formation of n type carbon nanotube array, the p-type carbon
Electrode is provided with nano-tube array and n type carbon nanotube array.
Further, the substrate is flexible polymethyl methacrylate (PMMA), the p-type carbon nano pipe array and
The electrode set on n type carbon nanotube array is silver electrode, is obtained by conductive silver paste solidification.
The flexible infrared sensor based on carbon nano pipe array that the present invention is provided, is followed successively by polymethyl from the bottom up
Sour methyl esters substrate, p-type carbon nano pipe array and n type carbon nanotube array, the p-type carbon nano pipe array and n type carbon nanotube
Silver electrode is provided with array.
Present invention also offers a kind of flexible infrared sensor based on carbon nano pipe array, poly- first is followed successively by from the bottom up
Base methyl acrylate substrate, n type carbon nanotube array and p-type carbon nano pipe array, the p-type carbon nano pipe array and N-type carbon
Silver electrode is provided with nano-tube array.
P-type carbon nano pipe array and N-type carbon in the flexible infrared sensor based on carbon nano pipe array that the present invention is provided
Nano-tube array forms the built in field for having N to point to P between P-N junction, P-N junction, when the flexible infrared sensor is by infrared
During light irradiation, the unnecessary carrier of generation can be moved in the presence of built in field, and wherein electronics flows to N sides, hole
P sides are flowed to, it is outside then p-type carbon nano pipe array and N-type can be passed through so as to there occurs the change of phase boundary potential on P-N junction surface
Silver electrode on carbon nano pipe array detects voltage.
Embodiment
Present invention also offers a kind of preparation method of the flexible infrared sensor based on carbon nano pipe array, including it is following
Step：
Step 1：With polymethyl methacrylate (PMMA) for solute, methyl phenyl ethers anisole is solvent, prepares mass concentration and is
The methyl phenyl ethers anisole solution of 0.08g/mL polymethyl methacrylate；
Step 2：Prepare p-type carbon nano pipe array：Silicon dioxide substrates are respectively washed 3 times, nitrogen in acetone and alcohol
It is standby after air-blowing is dry；Then using ferrocene as solute, toluene is solvent, and the toluene for preparing mass fraction for 3% ferrocene is molten
Liquid is used as precursor liquid；Silicon dioxide substrates after above-mentioned cleaning is dried up are put into tube furnace, with volume percentage purity
, then will with syringe for tubular type in-furnace temperature is increased into 850 DEG C by room temperature under 99.999% argon gas atmosphere, in 30min
The precursor liquid of above-mentioned preparation is injected into tube furnace, and the injection rate of precursor liquid is 10mL/h, and precursor liquid is heated to before injection
200℃；Then in 850 DEG C, the mixed-gas atmosphere of the hydrogen of the argon gas of 94% (percent by volume) and 6% (percent by volume)
Lower heat treatment 30min, makes CNT be grown in silicon dioxide substrates；After growth terminates, stop the injection of precursor liquid, make two
Oxidation silicon chip naturally cools to room temperature from 850 DEG C with stove, takes out substrate, i.e., p-type carbon nanometer is obtained in silicon dioxide substrates
Pipe array；
Step 3：Prepare n type carbon nanotube array：Silicon dioxide substrates are respectively washed 3 times, nitrogen in acetone and alcohol
It is standby after air-blowing is dry；Then using ferrocene as solute, acetonitrile and alcohol mixed solution are solvent, and it is 2% to prepare mass fraction
Solution of ferrocene is 16 as precursor liquid, the wherein mass ratio of acetonitrile and ethanol:1；Silica after above-mentioned cleaning is dried up
Substrate is put into tube furnace, by tube furnace under using volume percentage purity as 99.999% argon gas atmosphere, in 30min
Temperature be increased to 850 DEG C by room temperature, then the precursor liquid of above-mentioned preparation is injected into tube furnace with syringe, precursor liquid
Precursor liquid is heated to 250 DEG C before injection rate is 8mL/h, injection；Then in 850 DEG C, the argon gas of 94% (percent by volume)
30min is heat-treated with the mixed-gas atmosphere of the hydrogen of 6% (percent by volume), makes CNT in silicon dioxide substrates
Growth；After growth terminates, stop the injection of precursor liquid, silicon dioxide substrates is naturally cooled to room temperature from 850 DEG C with stove, take out
Substrate, i.e., obtain n type carbon nanotube array in silicon dioxide substrates；
Step 4：The poly- first that step 1 is prepared is dripped in the silicon dioxide substrates with p-type carbon nano pipe array that step 2 is obtained
The methyl phenyl ethers anisole solution of base methyl acrylate to whole covering substrates stop, and are put into 150 DEG C of baking 20min in baking oven, treat polymethyl
After sour methyl esters solidification, it is peeled off from substrate, the polymethyl methacrylate with p-type carbon nano pipe array is obtained, then will
Polymethyl methacrylate with p-type carbon nano pipe array is fitted tightly over the base with n type carbon nanotube array that step 3 is obtained
It is seamless between p-type carbon nano pipe array and n type carbon nanotube array to ensure on piece, the polymethylacrylic acid that drop step 1 is prepared
The methyl phenyl ethers anisole solution of methyl esters to whole covering substrates stop, and are put into 150 DEG C of baking 20min in baking oven, treat that polymethyl methacrylate coagulates
Gu after, it is peeled off from substrate, i.e., the p-type carbon nano pipe array being laminated from the bottom up on polymethyl methacrylate
With n type carbon nanotube array；
Step 5：Silver paste is put on the p-type carbon nano pipe array and n type carbon nanotube array obtained in step 4, and at 120 DEG C
Lower baking 20min, solidifies silver paste, obtains silver electrode on p-type carbon nano pipe array and n type carbon nanotube array, that is, completes base
In the making of the flexible infrared sensor of carbon nano pipe array.
Fig. 1 is the structural representation for the flexible infrared sensor based on carbon nano pipe array that the embodiment of the present invention is obtained.
Fig. 2 is the scanning electron microscope diagram (SEM) for the carbon nano pipe array that the embodiment of the present invention is prepared.Wherein, (a) is p-type
The scanning electron microscope (SEM) photograph of carbon nano pipe array, (b) is the scanning electron microscope (SEM) photograph of n type carbon nanotube array.As shown in Figure 2, embodiment into
Work(has prepared the CNT of array arrangement, and the diameter of n type carbon nanotube is bigger than p-type CNT.
Fig. 3 is the x-ray photoelectron energy spectrum diagram (XPS) for the n type carbon nanotube array that the embodiment of the present invention is obtained.By Fig. 2
Understand, the embodiment of the present invention successfully enters nitrogen-doping in CNT, has obtained n type carbon nanotube array.
Fig. 4 is the obtained flexible infrared sensor based on carbon nano pipe array of the embodiment of the present invention in 850nm wavelength
Response curve.Test process is：At room temperature, two electrode (p-types of the flexible infrared sensor embodiment of the present invention obtained
Silver electrode on carbon nano pipe array and n type carbon nanotube array) Agilent B2901A sources table is connected to, then using periodically
Wavelength be 850nm Infrared irradiation sensor, pass through source table read both end voltage change.As shown in Figure 4, prepare at room temperature
The flexible infrared sensor of carbon nano pipe array have obvious response to infrared.Flexible infrared sensor prepared by the present invention is logical
Cross test P-N junction open-circuit voltage to characterize infrared response, the power consumption of sensor is extremely low, but response is obvious；The lining that the present invention is used
Bottom polymethyl methacrylate has good flexibility, and the infrared-sensitive material carbon nano-pipe array of use is listed in when substrate is bent not
It can damage so that the sensor of preparation is flexible and stability is good.
Claims (6)
1. a kind of preparation method of the flexible infrared sensor based on carbon nano pipe array, comprises the following steps：
Step 1：Prepare methyl phenyl ethers anisole solution of the mass concentration for 0.08g/mL polymethyl methacrylate；
Step 2：P-type carbon nano pipe array and n type carbon nanotube array are prepared using floating catalytic chemical vapour deposition technique respectively；
Step 3：The polymethyl methacrylate that step 1 is prepared is dripped on the substrate with p-type carbon nano pipe array that step 2 is obtained
Methyl phenyl ethers anisole solution to whole covering substrates stop, be put into baking oven and dry, after after polymethyl methacrylate solidification, by it from base
Peeled off on piece, obtain the polymethyl methacrylate with p-type carbon nano pipe array, then will be poly- with p-type carbon nano pipe array
Methyl methacrylate is fitted tightly on the substrate with n type carbon nanotube array that step 2 is obtained to ensure p-type CNT
Seamless between array and n type carbon nanotube array, the methyl phenyl ethers anisole solution for the polymethyl methacrylate that drop step 1 is prepared is to whole
Covering substrate stops, and is put into baking oven and dries, and after after polymethyl methacrylate solidification, it is peeled off from substrate, i.e., in poly- first
The p-type carbon nano pipe array and n type carbon nanotube array being laminated on base methyl acrylate；
Step 4：Electrode is prepared on the p-type carbon nano pipe array and n type carbon nanotube array obtained in step 3.
2. the preparation method of the flexible infrared sensor according to claim 1 based on carbon nano pipe array, its feature exists
In the temperature when methyl phenyl ethers anisole solution that drop has polymethyl methacrylate is dried described in step 3 is 150 DEG C, drying time
For 20min；The electrode prepared described in step 4 on p-type carbon nano pipe array and n type carbon nanotube array is silver electrode, is led to
Conductive silver paste solidification is crossed to obtain.
3. a kind of preparation method of the flexible infrared sensor based on carbon nano pipe array, comprises the following steps：
Step 1：Prepare methyl phenyl ethers anisole solution of the mass concentration for 0.08g/mL polymethyl methacrylate；
Step 2：P-type carbon nano pipe array and n type carbon nanotube array are prepared using floating catalytic chemical vapour deposition technique respectively；
Step 3：The polymethyl methacrylate that step 1 is prepared is dripped on the substrate with n type carbon nanotube array that step 2 is obtained
Methyl phenyl ethers anisole solution to whole covering substrates stop, be put into baking oven and dry, after after polymethyl methacrylate solidification, by it from base
Peeled off on piece, obtain the polymethyl methacrylate with n type carbon nanotube array, then will be poly- with n type carbon nanotube array
Methyl methacrylate is fitted tightly on the substrate with p-type carbon nano pipe array that step 2 is obtained to ensure n type carbon nanotube
Seamless between array and p-type carbon nano pipe array, the methyl phenyl ethers anisole solution for the polymethyl methacrylate that drop step 1 is prepared is to whole
Covering substrate stops, and is put into baking oven and dries, and after after polymethyl methacrylate solidification, it is peeled off from substrate, i.e., in poly- first
The n type carbon nanotube array and p-type carbon nano pipe array being laminated on base methyl acrylate；
Step 4：Electrode is prepared on the n type carbon nanotube array and p-type carbon nano pipe array obtained in step 3.
4. the preparation method of the flexible infrared sensor according to claim 3 based on carbon nano pipe array, its feature exists
In the temperature when methyl phenyl ethers anisole solution that drop has polymethyl methacrylate is dried described in step 3 is 150 DEG C, drying time
For 20min；The electrode prepared described in step 4 on n type carbon nanotube array and p-type carbon nano pipe array is silver electrode, is led to
Conductive silver paste solidification is crossed to obtain.
5. the preparation side of the flexible infrared sensor according to any one of claim 1 to 4 based on carbon nano pipe array
Method, it is characterised in that the preparation process of p-type carbon nano pipe array described in step 2 is：Using ferrocene as solute, toluene is molten
Agent, the toluene solution for preparing mass fraction for 3% ferrocene is used as precursor liquid；Silicon dioxide substrates are placed in tube furnace,
Tubular type in-furnace temperature is heated to 850 DEG C under an argon atmosphere, the precursor liquid of above-mentioned preparation is then injected with 10mL/h speed,
30min is heat-treated under 850 DEG C, the mixed-gas atmosphere of argon gas and hydrogen, CNT is grown in silicon dioxide substrates；
After heat treatment terminates, room temperature is naturally cooled to stove under an argon atmosphere, i.e., p-type CNT is obtained in silicon dioxide substrates
Array.
6. the preparation side of the flexible infrared sensor according to any one of claim 1 to 4 based on carbon nano pipe array
Method, it is characterised in that the preparation process of n type carbon nanotube array described in step 2 is：Using ferrocene as solute, acetonitrile and second
Mixed alkoxide solution is solvent, prepare mass fraction for 2% solution of ferrocene as precursor liquid, wherein acetonitrile and ethanol quality
Than for 16:1；Silicon dioxide substrates are placed in tube furnace, tubular type in-furnace temperature 850 DEG C are heated under an argon atmosphere, so
The precursor liquid of above-mentioned preparation is injected with 8mL/h speed afterwards, is heat-treated under 850 DEG C, the mixed-gas atmosphere of argon gas and hydrogen
30min, makes CNT be grown in silicon dioxide substrates；After heat treatment terminates, naturally cooled under an argon atmosphere with stove
Room temperature, i.e., obtain n type carbon nanotube array in silicon dioxide substrates.
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| CN110885059B (en) * | 2019-04-23 | 2023-05-09 | 厦门大学 | Power generation method of carbon nano tube array |
| CN111735379B (en) * | 2020-05-15 | 2021-06-08 | 吉林大学 | Coated bionic flexible sensor for multi-mode information measurement |
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