CN109825816A - A kind of molybdenum disulfide film gas sensitive and preparation method and application - Google Patents
A kind of molybdenum disulfide film gas sensitive and preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of molybdenum disulfide film gas sensitives and its preparation method and application.The MoS that the gas sensitive uses CVD method to obtain2Thin-film material.Firstly, using electron beam evaporation plating with the deposition rate of 0.1A/s in SiO2The certain thickness molybdenum atom layer of preplating on/Si substrate；Then, MoS is generated by CVD method and S steam generation combination reaction under certain temperature2Film gas-sensitive material.The surface of acquisition is grown into MoS2The substrate both ends of nanometer sheet plate gold electrode respectively；Conductive silver glue is reused by conducting wire and gold electrode adhesion, is finally fixed using insulation AB glue to increase the intensity of air-sensitive test device, aging and encapsulation is carried out to test device, to obtain NO2The preparation of gas sensor.Gas sensor obtained by the present invention can realize room temperature to NO2The detection of gas, low energy consumption, and selectively good to interference gas, to NO2Gas has important meaning in terms of being monitored in real time.
Description
Technical field
The invention belongs to technical field of nano material, are related to a kind of for detecting NO2The MoS of gas2Film gas-sensitive material,
More particularly to a kind of molybdenum disulfide film gas sensitive and preparation method and application.
Technical background
Molybdenum disulfide (MoS2) it is a kind of transition metal dichalcogenide, it is widely used in solid lubrication, catalyst, too
Positive energy battery and sensor etc. fields.The two-dimentional MoS of the single layer of class graphene or few layer2Not only there is layer similar with graphene
Shape structure also possesses regulatable band gap, excellent optically and electrically performance is shown, in physics, chemistry, material, electricity
The fields such as son suffer from huge application potential.Single layer or few layer MoS are prepared at present2There are two main classes for the approach of film: from upper
And down and from bottom to top.It is the MoS with multilayered structure from top to bottom2As raw material, using micromechanics stripping method, lithium ion intercalation
Method, laser thinning method etc. prepare the less MoS of the number of plies2.Another kind of bottom-to-top method is anti-by chemistry by other substances
Two-dimensional MoS should be synthesized2, there are commonly chemical vapor deposition (CVD) methods.
MoS2Preparation and in gas sensing field, application has achieved more research achievement, but still asked there are some
It inscribes urgently to be resolved, is mainly manifested in the following aspects:
(1) two dimension MoS2It is poor to the selectivity of under test gas, it is lower for complicated gaseous environment detection accuracy；
(2) two dimension MoS2Controllability is poor on growth quality and growth area, and growth district is smaller, not can guarantee region
The uniformity of interior thickness and the consistency of the number of plies；
(3) most gas sensors need to work at a certain temperature, and power consumption is higher.
Summary of the invention:
The purpose of the present invention is to provide a kind of large area, few layer two dimension MoS2The preparation method of thin-film material, will be this
Material is fabricated to gas sensitive device for NO2The room temperature of gas detects, and the gas sensor which obtains is for NO2Gas has spirit
The performance of the excellent air-sensitives such as sensitivity is higher, selectivity is good, stability is good, room temperature detection.
An object of the present invention is to provide a kind of few layer two dimension MoS2Gas sensitive.
The second object of the present invention is to provide a kind of few layer two dimension MoS2The preparation method of gas sensitive.
The third object of the present invention is to provide a kind of few layer two dimension MoS2The gas sensor of gas sensitive.
The fourth object of the present invention is to provide a kind of few layer two dimension MoS2The gas sensor production method of gas sensitive.
The fifth object of the present invention is to provide a kind of few layer two dimension MoS2Gas sensitive and preparation method thereof, few layer two dimension
MoS2The application of the sensor of gas sensitive.
To achieve the above object, the invention provides the following technical scheme:
One kind is based on few layer two dimension MoS2The production method of sensitive material and sensing element, the MoS2Sensitive material is served as reasons
Chemical vapour deposition technique (CVD) preparation is grown in SiO2Two-dimentional MoS on/Si substrate2Material is made by including the following steps
It is standby to form:
Step 1: using electron beam evaporation plating in 0.1-1.5cm2The SiO of size2The molybdenum of preplating different-thickness is former on/Si substrate
Sublayer, the electron beam evaporation plating are the deposition rates with 0.1A/s in SiO2Molybdenum atom layer is deposited on/Si substrate；It is above-mentioned to be adopted
SiO2/ Si substrate SiO2With a thickness of 300nm.
Step 2: Massive Sulphur grind into powder is laid in porcelain boat, and the Massive Sulphur is that purity is 99.99%
High purity sulphur；The porcelain boat, also known as burning ship, combustion boat, are a kind of chemical porcelains, specification: 72mm, 77mm, 88mm, 95mm, 97mm,
Selected porcelain boat dimensions is selected according to actual production demand in the present invention.
Step 3: the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in the quartz ampoule in tube furnace, and adjusts position
It sets；The porcelain boat position is the uptake in diamond heating region, and makes the holding in reaction of its temperature by adjusting position
At 200~300 DEG C；
Step 4: the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed
In tube furnace center constant temperature zone；
Step 5: leading to high-purity argon gas first to empty inner air tube, be then changed to logical high pure nitrogen in Xiang Shangshu CVD system,
Tube furnace starts to carry out-the temperature-fall period that heats up-keep the temperature according to the temperature program(me) set while logical nitrogen, is made described and is used for
NO2The MoS of gas efficient detection2Gas sensor；The CVD system that the CVD system is voluntarily built for laboratory, including one
Platform can accurately control reaction temperature, heating, the tubular heater of soaking time and a set of control reaction process in experiment
In be passed through the flow control system of gas flow amount；
According to reactionTo carry out reaction forward, guarantee sufficient S, in the step 2
The quality of sulphur is no less than 0.8g.
Wherein, described flow velocity when being passed through gas with various is different, is when being first passed through high-purity argon gas into quartz ampoule respectively
Flow velocity is 100sccm, and flow velocity when being passed through high pure nitrogen is 50sccm；
Wherein, the CVD temperature program(me) system is that 20min is warming up to 200 DEG C, keep the temperature and be warming up to 650 after 20min~
850 DEG C, 0~60min is kept the temperature, after reaction Temperature fall.
One kind is for detecting NO2The MoS of gas2Application of the film gas-sensitive material in terms of preparing gas sensor, the air-sensitive
The preparation method of element includes the following steps:
The surface of above-mentioned acquisition is grown into MoS2The SiO of nanometer sheet2/ Si substrate two sides plate gold electrode respectively；
Conductive silver glue is reused by conducting wire and gold electrode adhesion；
It is further fixed after conductive silver glue substantially dry ready for use using insulation AB glue, increases air-sensitive tester
The intensity of part.The insulation AB glue is two liquid mixed hardening glue of insulation.
The AB glue is the nickname of two liquid mixed hardening glue, and a liquid is this glue, and a liquid is curing agent, and two liquid phases are mixed could be hard
Change, is not necessary to answer maturation firmly by temperature, so being one kind of cold(-)setting glue, makees model and use sometimes.
AB glue is the call of two component adhesive.The commercially available AB glue for having the ingredients such as acrylic acid, epoxy, polyurethane.
AB glue has very high adhesive strength, but there is also some shortcomings, as curing time is long, manual mixing is irregular
Cause to solidify bad, smell than heavier etc. deficiency.There is a set of quick dispenser system can solve at present, this system is in foreign countries
Popularized, at home there are no universal, most people using when use conventional methods and carry out dispensing gluing.This set
System is mainly made of glue gun, two-component syringe, mixing tube three big parts.Glue factory is pre- by AB glue using two-component syringe
First packing and storing is inside AB glue syringe, when use above glue gun, then mixing tube is connect in the upper surface of gum outlet,
Using the mixing hinge inside mixing tube by two kinds of glue mixing tubes uniformly (after general 7 section can, use it is mostly be 17
Section, hundred times of the mixed effect quite with craft), then glue is coated onto the position for needing to be bonded.General dispenser system is
It is not the AB glue of bonding for bringing the AB glue of the cementation of fissures.
The chemical vapor deposition (CVD) is the skill for depositing multiple materials being most widely used in semi-conductor industry
Art, including large-scale insulating materials, most metals material and metal alloy compositions.In theory: two kinds or two kinds
Above gaseous starting materials are imported into a reaction chamber, and then they chemically react between each other, are formed a kind of new
Material deposits in wafer surface.Silicon nitride film (Si3N4) is exactly a good example, it is anti-by silane and nitrogen
It should be formed.
Reaction in reaction chamber be it is very complicated, have the factor that much must be taken into consideration, the variation range of deposition parameter is very
It is wide: react indoor pressure, the temperature of chip, the flow rate of gas, gas by the distance of chip, gas chemistry at
Whether part, a kind of gas phase for the ratio of another gas, the intermediate products role of reaction and need other reactions
Outdoor external energy source accelerates or induces conceivable reaction etc..Additional energy source such as energy of plasma, certainly
A whole set of new parameter can be generated, such as the ratio of ion and neutral gas flow, ion can be with the rf bias etc. on chip.On the other hand
It need to consider the parameter in deposition film: as (the latter refers to for the uniformity of thickness and the coverage property on figure in whole chip
Covering across figure step), the stoicheiometry (chemical analysis and distribution) of film crystallizes crystal orientation and defect concentration etc..When
So, deposition rate is also an important factor because it decides the quantum of output of reaction chamber, high deposition rate be often required to and
The high quality of film, which is compromised, to be considered.The film that reaction generates can be not only deposited on chip, can also be deposited on other portions of reaction chamber
On part, the number and thorough degree cleaned to reaction chamber is also critically important.
Chemical vapour deposition technique is traditional technology for preparing film, and principle is led to using gaseous pioneer's reactant
Atom, intermolecular chemical reaction are crossed, so that certain ingredient breakdowns in gaseous precursor, and film is formed on matrix.Chemistry
Vapor deposition includes aumospheric pressure cvd, plasma auxiliary chemical deposition, Laser-assisted chemical deposition, Organometallic
Close object deposition etc..
The present invention passes through in SiO2/ Si substrate surface deposits MoS2Few layer film, utilizes MoS2Film is to NO2Absorption, grind
Producing has to NO2The MoS of sensitlzing effect2Thin-film device.The operating condition of device involved in the present invention is eliminated to heating condition
With the dependence of noble metal, preparation method is simple, low in cost, and has NO2Response performance is significant, reproducible, reliable
The advantages that property is high, can be widely applied to NO2Detection field.
Compared with prior art, of the invention to have the advantages that
(1) one kind is provided in SiO2/ Si substrate prepares single layer or few layer MoS2Preparation method；
(2) a kind of production method that the gas sensitive being grown directly upon on substrate is made into air-sensitive test device is provided；
(3) using electron beam evaporation plating in SiO2For preplating molybdenum atom layer on/Si substrate as molybdenum source, sulphur powder is sulphur source；
(4) simple process, cost is relatively low and not can cause environmental pollution；
(5) gas sensor is at room temperature to NO2Gas has preferable sensitive property, and prepared molybdenum disulfide is at room temperature
To the NO of 100ppm concentration2Gas sensitivity is respectively 31.3%, and response time 4s, recovery time 5s, sensitivity is higher,
It is very fast to respond resume speed.
Detailed description of the invention
Fig. 1 is two dimension MoS in the embodiment of the present invention 12Fluorescence (PL) spectrum of gas sensitive；
Fig. 2 is two dimension MoS in the embodiment of the present invention 12The Raman spectrogram of gas sensitive；
Fig. 3 is two dimension MoS in the embodiment of the present invention 12The optical microscope of gas sensitive；
Fig. 4 is gas sensor in the embodiment of the present invention 1 to 100ppmNO2Response recovery curve figure；
Fig. 5 is gas sensor in the embodiment of the present invention 1 to the selective figure of interference gas；
Fig. 6 is gas sensor in the embodiment of the present invention 1 to various concentration NO2The linear relationship chart of gas response；
Fig. 7 is gas sensor element schematic of the present invention.
Specific embodiment
Keep the contents of the present invention more clear and easy to understand, below in conjunction with Figure of description, the contents of the present invention is made further
Explanation.Certainly the invention is not limited to the specific embodiment, and general replacement known to those skilled in the art is also contained
Lid is within the scope of the present invention.
Embodiment 1:
One kind is for detecting NO2The MoS of gas2Film gas-sensitive material and preparation method thereof, the preparation method include following step
It is rapid:
1, the MoS of single layer or few layer is prepared using CVD method2Film gas-sensitive material；
Above-mentioned is grown in SiO2The MoS of/Si substrate surface2Sensitive material area about 0.25cm2, the two-dimentional MoS2
Gas sensitive preparation method:
1. using electron beam evaporation plating in SiO2Preplating obtains the molybdenum layer of 1nm thickness, the electron beam evaporation plating on/Si substrate
It is to be plated on substrate with the deposition rate of 0.1A/s, above-mentioned used SiO2SiO in/Si substrate2Layer with a thickness of 300nm.
2. Massive Sulphur grind into powder is laid in porcelain boat, the Massive Sulphur is the height that 0.8g purity is 99.99%
Bright sulfur；
3. the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in tube furnace, and temperature is adjusted, the porcelain boat is placed in
Tube furnace is placed in the uptake in diamond heating region, and so that the temperature of sulphur is maintained at 260 in reaction by adjusting temperature
℃；
4. the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed in tubular type
Furnace center constant temperature zone；
5. leading to high-purity argon gas first into above-mentioned CVD system to empty inner air tube, it is then changed to logical high pure nitrogen, leads to nitrogen
While tube furnace start to carry out-the temperature-fall period that heats up-keep the temperature according to the temperature program(me) set, be made described for efficiently examining
Survey NO2The two-dimentional MoS of gas2Gas sensitive；
Wherein, described flow velocity when being passed through gas with various is different, is when being first passed through high-purity argon gas into quartz ampoule respectively
Flow velocity is 100sccm, and flow velocity when being passed through high pure nitrogen is 50sccm；The CVD temperature program(me) system is warming up to for 20min
200 DEG C, 750 DEG C are warming up to after keeping the temperature 20min, keeps the temperature 30min, after reaction Temperature fall.
The HREvolution spectrometer produced using Japanese HORIBA company, to above-mentioned resulting two dimension MoS2Air-sensitive material
Material is measured, and resulting fluorescence spectra is as shown in Figure 1, from the map, it can be seen that sample crystallization obtained by under the experiment condition
Preferably；Raman spectrogram keeps the temperature the sample A of 30min as shown in Figure 21 g-E1 2g=23.64, corresponding gained sample is 3 layers of two dimension
MoS2。
Optical microscopy provisioned in HREvolution spectrometer using the production of Japanese HORIBA company, to above-mentioned reality
It applies gas sensitive obtained in example 1 to be characterized, gained optical microscope is as shown in figure 3, sample table obtained by when keeping the temperature 30min
Face is uniform.
Fig. 4 is the NO of soaking time obtains after being 30min after being warming up to 750 DEG C gas sensor to 100ppm concentration2's
Recovery curve figure is responded, the experimental results showed that, sensitivity is higher, and response resume speed is very fast.
Fig. 5 is gas sensor made by soaking time obtains after being 30min after being warming up to 750 DEG C gas sensitive to dry
Disturb the selective figure of gas；Ethyl alcohol, methanol that concentration is 100ppm, acetone, formaldehyde, NO are passed through into chamber to be measured2And ammonia
6 kinds of gas with various of gas, survey its sensitivity, it can be deduced that prepared MoS respectively2For NO2There is higher sensitivity, it is prepared
Molybdenum disulfide gas sensor at room temperature to the NO of 100ppm concentration2Gas sensitivity (- Δ R/R, unit %) is respectively
31.3%, and to remaining four kinds of gas without obvious responsing to.
Fig. 6 is gas sensor made by soaking time obtains after being 30min after being warming up to 750 DEG C gas sensitive to not
With concentration NO2The linear relationship chart of gas response；For 100ppmNO2Test under the various concentration that air-sensitive performance carries out, then
The matched curve for carrying out sensitivity and concentration takes logarithm simultaneously to two reference axis, obtains the logarithm of concentration and the logarithm of sensitivity
It is in a linear relationship, it can be expressed as lg (s)=0.16+0.69lg (c), wherein s and c respectively represent sensitivity and gas concentration.
Air-sensitive test is carried out using the CGS-1TP intelligence air-sensitive analysis system of Beijing Ai Lite Science and Technology Ltd. production,
Its airtight chamber with 24L can carry out air-sensitive test.Test method is to pass through a certain amount of configured test solution
Micro syringe is injected on the indoor evaporator of chamber, is sufficiently uniformly dispersed in chamber after evaporating solution.
2, as shown in fig. 7, it is a kind of for detecting NO2The MoS of gas2Film gas-sensitive material is preparing gas sensor, including AB
Glue (half-sectional) 1, conducting wire 2, two dimension MoS2Substrate 3, conductive silver glue and gold electrode 4, structure is simple, easy for installation, improves detection effect
Rate.Its preparation process is as follows:
Surface obtained above is grown into two dimension MoS23 both ends of substrate plate gold electrode 4 respectively；Reuse conductive silver glue
By 4 adhesion of conducting wire 2 and gold electrode；It is further fixed after conductive silver glue is dry using the AB glue (half-sectional) 1 of insulation, to improve air-sensitive
Test the bond strength of device.
Embodiment 2:
One kind is for detecting NO2The MoS of gas2Film gas-sensitive material and preparation method thereof, the preparation method include following step
It is rapid:
1, the MoS of single layer or few layer is prepared using CVD method2Film gas-sensitive material；
The above-mentioned sensitive material area for being grown in substrate surface is about the size of a substrate, is 0.1cm2, described
Two-dimentional MoS2Nanometer sheet is prepared by a method comprising the following steps:
1. using electron beam evaporation plating in SiO2Preplating obtains the molybdenum atom layer of 1nm thickness, the electron beam on/Si substrate
Vapor deposition is plated on substrate with the deposition rate of 0.1A/s, above-mentioned used SiO2/ Si substrate with a thickness of 300nm.
2. Massive Sulphur grind into powder is laid in porcelain boat, the Massive Sulphur is the height that 0.8g purity is 99.99%
Bright sulfur；
3. the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in tube furnace, and temperature is adjusted, the porcelain boat is placed in
Tube furnace is placed in the uptake in diamond heating region, and so that the temperature of sulphur is maintained at 200 in reaction by adjusting temperature
℃；
4. the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed in tubular type
Furnace center constant temperature zone
5. leading to high-purity argon gas first into above-mentioned CVD system to empty inner air tube, it is then changed to logical high pure nitrogen, leads to nitrogen
While tube furnace start to carry out heating and heat preservation temperature-fall period according to the temperature program(me) that sets, be made described and be used for efficient detection
NO2The two-dimentional MoS of gas2Nanometer sheet；The CVD system is the CVD system that laboratory is voluntarily built, including one can essence
Really gas is passed through in the reaction temperature in control experiment, heating, the tubular heater of soaking time and a set of control reaction process
The flow control system of body throughput；Wherein,
Described flow velocity when being passed through gas with various is different, is that flow velocity is when being first passed through high-purity argon gas into quartz ampoule respectively
100sccm, flow velocity when being passed through high pure nitrogen are 50sccm；
The CVD temperature program(me) system is that 20min is warming up to 200 DEG C, 750 DEG C of reaction temperature is raised to after 20min, reaction
After Temperature fall.
2, as shown in fig. 7, it is a kind of for detecting NO2The MoS of gas2Film gas-sensitive material is preparing gas sensor, including AB
Glue (half-sectional) 1, conducting wire 2, two dimension MoS2Substrate 3, conductive silver glue and gold electrode 4, structure is simple, easy for installation, improves detection effect
Rate.Its preparation process is as follows:
Surface obtained above is grown into two dimension MoS23 both ends of substrate plate gold electrode 4 respectively；Reuse conductive silver glue
By 4 adhesion of conducting wire 2 and gold electrode；It is further fixed after conductive silver glue is dry using the AB glue (half-sectional) 1 of insulation, to improve air-sensitive
Test the bond strength of device.
Embodiment 3:
One kind is for detecting NO2The MoS of gas2Film gas-sensitive material and preparation method thereof, the preparation method include following step
It is rapid:
1, the MoS of single layer or few layer is prepared using CVD method2Film gas-sensitive material；
The above-mentioned sensitive material area for being grown in substrate surface is about the size of a substrate, is 1cm2, described two
Tie up MoS2Nanometer sheet is prepared by a method comprising the following steps:
1. using electron beam evaporation plating in SiO2Preplating obtains the molybdenum atom layer of 1nm thickness, the electron beam on/Si substrate
Vapor deposition is plated on substrate with the deposition rate of 0.1A/s, above-mentioned used SiO2/ Si substrate with a thickness of 300nm.
2. Massive Sulphur grind into powder is laid in porcelain boat, the Massive Sulphur is the height that 0.8g purity is 99.99%
Bright sulfur.
3. the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in tube furnace, and temperature is adjusted, the porcelain boat is placed in
Tube furnace is placed in the uptake in diamond heating region, and so that the temperature of sulphur is maintained at 300 in reaction by adjusting temperature
℃。
4. the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed in tubular type
Furnace center constant temperature zone.
5. leading to high-purity argon gas first into above-mentioned CVD system to empty inner air tube, it is then changed to logical high pure nitrogen, leads to nitrogen
While tube furnace start to carry out heating and heat preservation temperature-fall period according to the temperature program(me) that sets, be made described and be used for efficient detection
NO2The two-dimentional MoS of gas2Nanometer sheet；Described flow velocity when being passed through gas with various is different, is first to be passed through into quartz ampoule respectively
Flow velocity is 100sccm when high-purity argon gas, and flow velocity when being passed through high pure nitrogen is 50sccm；The CVD temperature program(me) system is
20min is warming up to 200 DEG C, is warming up to 750 DEG C after keeping the temperature 20min, keeps the temperature 60min, after reaction Temperature fall.
2, as shown in fig. 7, it is a kind of for detecting NO2The MoS of gas2Film gas-sensitive material is preparing gas sensor, including AB
Glue (half-sectional) 1, conducting wire 2, two dimension MoS2 substrate 3, conductive silver glue and gold electrode 4, structure is simple, easy for installation, improves detection effect
Rate.Its preparation process is as follows:
Surface obtained above is grown into two dimension MoS23 both ends of substrate plate gold electrode 4 respectively；Reuse conductive silver glue
By 4 adhesion of conducting wire 2 and gold electrode；It is further fixed after conductive silver glue is dry using the AB glue (half-sectional) 1 of insulation, to improve air-sensitive
Test the bond strength of device.
Embodiment 4:
One kind is based on few layer two dimension MoS2Sensitive material and be used for NO2The production method of the sensing element of gas detection, specifically
It is prepared by a method comprising the following steps:
1, few layer of the two-dimentional MoS prepared using indirect CVD method2Nanometer sheet is directly grown on substrate surface；
The above-mentioned sensitive material area for being grown in substrate surface is about the size of a substrate, is 0.25cm2, described
Two-dimentional MoS2Nanometer sheet is prepared by a method comprising the following steps:
1. using electron beam evaporation plating in SiO2Preplating obtains the molybdenum atom layer of 1nm thickness, the electron beam on/Si substrate
Vapor deposition is plated on substrate with the deposition rate of 0.1A/s；Used SiO2/ Si substrate with a thickness of 300nm.
2. Massive Sulphur grind into powder is laid in porcelain boat, the Massive Sulphur is the height that 0.9g purity is 99.99%
Bright sulfur；
3. the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in tube furnace, and temperature is adjusted, the porcelain boat is placed in
Tube furnace is placed in the uptake in diamond heating region, and so that the temperature of sulphur is maintained at 260 in reaction by adjusting temperature
℃；
4. the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed in tubular type
Furnace center constant temperature zone；
5. leading to high-purity argon gas first into above-mentioned CVD system to empty inner air tube, it is then changed to logical high pure nitrogen, leads to nitrogen
While tube furnace start to carry out-the temperature-fall period that heats up-keep the temperature according to the temperature program(me) set, be made described for efficiently examining
Survey NO2The two-dimentional MoS of gas2Gas sensitive；
Described flow velocity when being passed through gas with various is different, is that flow velocity is when being first passed through high-purity argon gas into quartz ampoule respectively
100sccm, flow velocity when being passed through high pure nitrogen are 50sccm；
The CVD temperature program(me) system is that 20min is warming up to 200 DEG C, is warming up to 650 DEG C after keeping the temperature 20min, heat preservation
30min, after reaction Temperature fall.
2, as shown in fig. 7, it is a kind of for detecting NO2The MoS of gas2Film gas-sensitive material is preparing gas sensor, including AB
Glue (half-sectional) 1, conducting wire 2, two dimension MoS2Substrate 3, conductive silver glue and gold electrode 4, structure is simple, easy for installation, improves detection effect
Rate.Its preparation process is as follows:
Surface obtained above is grown into two dimension MoS23 both ends of substrate plate gold electrode 4 respectively；Reuse conductive silver glue
By 4 adhesion of conducting wire 2 and gold electrode；It is further fixed after conductive silver glue is dry using the AB glue (half-sectional) 1 of insulation, to improve air-sensitive
Test the bond strength of device.
Embodiment 5:
One kind is for detecting NO2The MoS of gas2Film gas-sensitive material and preparation method thereof, the preparation method include following step
It is rapid:
1, the MoS of single layer or few layer is prepared using CVD method2Film gas-sensitive material；
The above-mentioned sensitive material area for being grown in substrate surface is about 1.5cm2Substrate on, the two-dimentional MoS2It receives
Rice piece, is prepared by a method comprising the following steps:
1. using electron beam evaporation plating in SiO2Preplating obtains the molybdenum atom layer of 1nm thickness on/Si substrate；The electron beam
Vapor deposition is plated on substrate with the deposition rate of 0.1A/s；SiO used by above-mentioned2/ Si substrate with a thickness of 300nm.
2. Massive Sulphur grind into powder is laid in porcelain boat, the Massive Sulphur is the height that 1.2g purity is 99.99%
Bright sulfur；
3. the porcelain boat that high-purity sulfur powder is expired in above-mentioned tiling is placed in tube furnace, and temperature is adjusted, the porcelain boat is placed in
Tube furnace is placed in the uptake in diamond heating region, and so that the temperature of sulphur is maintained at 260- in reaction by adjusting temperature
300℃；
4. the above-mentioned molybdenum base piece that plated face-up is placed on the card slot of quartz boat, above-mentioned quartz boat is placed in tubular type
Furnace center constant temperature zone；
5. leading to high-purity argon gas first into above-mentioned CVD system to empty inner air tube, it is then changed to logical high pure nitrogen, leads to nitrogen
While tube furnace start to carry out heating and heat preservation temperature-fall period according to the temperature program(me) that sets, be made described and be used for efficient detection
NO2The two-dimentional MoS of gas2Nanometer sheet；Wherein:
Described flow velocity when being passed through gas with various is different, is that flow velocity is when being first passed through high-purity argon gas into quartz ampoule respectively
100sccm, flow velocity when being passed through high pure nitrogen are 50sccm；
The CVD temperature program(me) system is that 20min is warming up to 200 DEG C, is warming up to 850 DEG C after keeping the temperature 20min, heat preservation
30min, after reaction Temperature fall.
2, as shown in fig. 7, it is a kind of for detecting NO2The MoS of gas2Film gas-sensitive material is preparing gas sensor, including AB
Glue (half-sectional) 1, conducting wire 2, two dimension MoS2Substrate 3, conductive silver glue and gold electrode 4, structure is simple, easy for installation, improves detection effect
Rate.Its preparation process is as follows:
3, surface obtained above is grown into two dimension MoS23 both ends of substrate plate gold electrode 4 respectively；Reuse conductive silver
Glue is by 4 adhesion of conducting wire 2 and gold electrode；It is further fixed after conductive silver glue is dry using the AB glue (half-sectional) 1 of insulation, to improve gas
The bond strength of quick test device.
It is research later period soaking time to MoS2The influence of synthesis, in tri- kinds of different heat preservations of 0min, 30min, 60min
Between under tested, the results showed that sample is best under 30min.Reaction just starts when keeping the temperature 0min, and crystal grain is not yet grown up completely；
After keeping the temperature 60min, since sulphur powder has been used up, reaction starts reverse progress, MoS2Almost decompose completely.Therefore, pass through setting
Different soaking times, it can proved responseAlso it can be concluded that when most preferably being kept the temperature in experimentation
Between.Reaction temperature determines the rate of molecular motion, has larger impact to the rate of reaction, is research reaction temperature to MoS2Synthesis
Influence, embodiment 1, example 4 are heat preservation 30min in example 5, and reaction temperature is respectively maintained at 750 DEG C, 650 in insulating process
℃,850℃.The experimental results showed that reaction rate is lower at 650 DEG C, Mo film not yet complete cure is at MoS2；And it is anti-at 850 DEG C
It answers temperature excessively high, reacts too fast, reaction balance is carried out to reverse after causing S to exhaust, finally without MoS2It generates.Therefore, it is reacting
It is experiment optimum condition under conditions of 750 DEG C of temperature, heat preservation 30min.
MoS of the present invention2Film gas-sensitive material is equipped with exhaust gas processing device during preparing gas sensor, such as Fig. 7 institute
Show, prevents pollution environment.
Above content is only the basic explanation under present inventive concept, and that technical solution according to the present invention is done is any etc.
Effect transformation, should all belong to protection scope of the present invention.
Claims (10)
1. one kind is for detecting NO2The MoS of gas2Film gas-sensitive material, which is characterized in that the MoS2Sensitive material is by changing
That learns vapour deposition process preparation is grown in SiO2Two-dimentional MoS on/Si substrate2Thin-film material, the two dimension MoS2It is tied for few layer
Structure, few layer is two layers, three layers or four layers.
2. as described in claim 1 for detecting NO2The MoS of gas2Film gas-sensitive material, which is characterized in that the two dimension
MoS2The area of sensitive material is by SiO2/ Si chip area determines that the size is in 0.1-1.5cm2。
3. as described in claim 1 for detecting NO2The MoS of gas2Film gas-sensitive material, which is characterized in that used
SiO2/ Si substrate SiO2With a thickness of 300nm.
4. a kind of be used to detect NO as described in claim 1-32The MoS of gas2The preparation method of film gas-sensitive material, it is special
Sign is, includes the following steps:
Step 1: using electron beam evaporation plating in SiO2Preplating molybdenum atom layer on/Si substrate；
Step 2: evenly laid out in porcelain boat by Massive Sulphur in being ground into powder in mortar；
Step 3: the porcelain boat for uniformly filling sulphur powder in step 2 is placed in diamond heating area uptake nozzle position, and is led to
Crossing adjustment position makes its reaction temperature be maintained at 200~300 DEG C；
Step 4: by the SiO of molybdenum atom layer of preplating obtained by step 12/ Si substrate is face-up placed in the card of customization quartz boat
On slot, customization quartz boat is placed in tube furnace center constant temperature zone；
Step 5: lead to high-purity argon gas first into CVD system to empty inner air tube, be then changed to logical high pure nitrogen, lead to nitrogen
Tube furnace starts successively to be heated up according to the temperature program(me) set, keep the temperature, hypothermic response simultaneously, is made described for detecting
NO2The MoS of gas2Film gas-sensitive material.
5. as claimed in claim 4 for detecting NO2The MoS of gas2The preparation method of film gas-sensitive material, which is characterized in that
Molybdenum atom layer in the step 1 is to be plated in SiO using electron beam evaporation plating with the deposition rate of 0.1A/s2On/Si substrate.
6. as claimed in claim 4 for detecting NO2The MoS of gas2The preparation method of film gas-sensitive material, which is characterized in that
The quality of sulphur is no less than 0.8g in the step 2.
7. as claimed in claim 4 for detecting NO2The MoS of gas2The preparation method of film gas-sensitive material, which is characterized in that
In the step 5, with when flow velocity be 100sccm high-purity argon gas 20min is passed through into pipe, with when flow velocity be 50sccm into pipe
High pure nitrogen is passed through until reaction terminates.
8. as claimed in claim 4 for detecting NO2The MoS of gas2The preparation method of film gas-sensitive material, which is characterized in that
In the step 5, the temperature program(me) of the tube furnace of setting is that 20min is warming up to 200 DEG C, keep the temperature and be warming up to 650 after 20min~
850 DEG C, 0~60min is kept the temperature, after reaction Temperature fall.
9. as claimed in claim 4 for detecting NO2The MoS of gas2The preparation method of film gas-sensitive material, which is characterized in that
CVD system used in the step 5 includes the reaction temperature that can accurately control in experiment, a heating, soaking time
The flow control system of gas flow is passed through in tubular heater and a set of control reaction process.
10. one kind is for detecting NO2The MoS of gas2Application of the film gas-sensitive material in terms of preparing gas sensor, feature exist
In the preparation method of the gas sensor includes the following steps:
A) it uses and is grown in SiO2Two-dimentional MoS on/Si substrate2Material is gas sensor substrate；
B) obtained gas sensor substrate both ends are plated into two gold electrodes, and is glued conducting wire and gold electrode using conductive silver glue
Even；
C) it is fixed after conductive silver glue used in above-mentioned steps b) is dry using insulation AB glue.
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| CN110530935A (en) * | 2019-08-31 | 2019-12-03 | 中国石油大学(华东) | The construction method of molybdenum-disulfide radical gas sensing array and its in SF6Application in the detection of gas decomposition components |
| CN110629195A (en) * | 2019-09-27 | 2019-12-31 | 扬州大学 | Method for constructing semiconductor and metal sulfide heterogeneous electrode by chemical vapor deposition method |
| CN110734092A (en) * | 2019-10-28 | 2020-01-31 | 华南师范大学 | monoatomic layer tungsten disulfide two-dimensional material and preparation method and application of reverse physical vapor deposition thereof |
| CN111398363A (en) * | 2020-04-29 | 2020-07-10 | 中国科学院上海硅酸盐研究所 | Formaldehyde gas sensor based on molybdenum disulfide and hydroxylamine and preparation method thereof |
| CN111398368A (en) * | 2020-04-30 | 2020-07-10 | 中国人民解放军陆军防化学院 | Nitrogen dioxide gas sensor based on molybdenum disulfide and preparation method |
| CN111398367A (en) * | 2020-04-30 | 2020-07-10 | 中国人民解放军陆军防化学院 | Method for improving molybdenum disulfide gas sensor by adopting niobium and sensing equipment |
| CN111398366A (en) * | 2020-04-30 | 2020-07-10 | 中国人民解放军陆军防化学院 | Method for improving molybdenum disulfide gas sensor by adopting vanadium and sensing equipment |
| CN113249685A (en) * | 2021-04-09 | 2021-08-13 | 杭州电子科技大学 | Preparation method of silver sulfide film gas sensor |
| CN113418552A (en) * | 2021-06-09 | 2021-09-21 | 海南大学 | Two-dimensional transition metal sulfide material flexible sensor and preparation method thereof |
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| CN110629195A (en) * | 2019-09-27 | 2019-12-31 | 扬州大学 | Method for constructing semiconductor and metal sulfide heterogeneous electrode by chemical vapor deposition method |
| CN110734092A (en) * | 2019-10-28 | 2020-01-31 | 华南师范大学 | monoatomic layer tungsten disulfide two-dimensional material and preparation method and application of reverse physical vapor deposition thereof |
| CN110734092B (en) * | 2019-10-28 | 2021-01-19 | 华南师范大学 | Tungsten disulfide two-dimensional material with monoatomic layer, preparation method and application of tungsten disulfide two-dimensional material by reverse physical vapor deposition |
| CN111398363A (en) * | 2020-04-29 | 2020-07-10 | 中国科学院上海硅酸盐研究所 | Formaldehyde gas sensor based on molybdenum disulfide and hydroxylamine and preparation method thereof |
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| CN111398367A (en) * | 2020-04-30 | 2020-07-10 | 中国人民解放军陆军防化学院 | Method for improving molybdenum disulfide gas sensor by adopting niobium and sensing equipment |
| CN111398368A (en) * | 2020-04-30 | 2020-07-10 | 中国人民解放军陆军防化学院 | Nitrogen dioxide gas sensor based on molybdenum disulfide and preparation method |
| CN111398368B (en) * | 2020-04-30 | 2023-11-07 | 中国人民解放军陆军防化学院 | Molybdenum disulfide-based nitrogen dioxide gas sensor and preparation method thereof |
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| CN111398366B (en) * | 2020-04-30 | 2024-01-30 | 中国人民解放军陆军防化学院 | Method for improving molybdenum disulfide gas sensor by adopting vanadium and sensing equipment |
| CN113249685A (en) * | 2021-04-09 | 2021-08-13 | 杭州电子科技大学 | Preparation method of silver sulfide film gas sensor |
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