CN107024516A - A kind of rhenium disulfide nano-chip arrays film adsorbed sensor and preparation method - Google Patents
A kind of rhenium disulfide nano-chip arrays film adsorbed sensor and preparation method Download PDFInfo
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- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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Abstract
The disclosure discloses a kind of rhenium disulfide nano-chip arrays film adsorbed sensor and preparation method, and the sensor includes two parts of electrode basement and sensitive material.Electrode basement is made up of gold electrode and ceramic insulation sheet substrate, wherein, the gold electrode is interdigitated electrode structure.Sensitive material is rhenium disulfide nano-chip arrays film, is synthesized using chemical vapour deposition technique.By designing synthesis strategy, the rhenium disulfide nano-chip arrays film for obtaining and being orientated perpendicular to electrode basement can be deposited directly in electrode basement, to constitute adsorbed sensor.The sensor construction is simple, small volume, prepare that cost is low, synthesis is simple.Vertical orientated due to nanometer sheet, its surface can adsorb more gas molecules, and be conducive to the diffusion of molecule.Therefore, compared to existing sensor, it has the advantages that sensitivity is high, response recovery time is short, accuracy is good, is especially suitable for popularization and application.
Description
Technical field
This disclosure relates to micro-nano gas sensing field, more particularly to a kind of absorption of rhenium disulfide nano-chip arrays film
Formula sensor and preparation method.
Background technology
In recent years, developed rapidly the need for being detected with every profession and trade field gas with micro-nano manufacturing technology, nanometer is passed
Sensor will play the part of important role in terms of following gaseous detection applications.Transition-metal dichalcogenide (TMDs) possesses solely
Special electrical and optical properties, per layer material are combined together by weak interactions such as Van der Waals fors, and it is constructed
Two-dimension nano materials can be by mechanically pulling off or chemical vapour deposition technique obtain, with excellent absorption, conductive characteristic,
Fabulous application prospect is shown in micro-nano gas sensor domain.The principle of adsorbed sensor is when gas molecule absorption
During to sensitive material surface, hybridized orbit can be formed between gas molecule and material, its surface energy band is bent, causes electric charge
Transfer, and then change the distribution of charges of material, macroscopically showing as the change of the electrical parameters such as electric capacity or conductance.Gas concentration is just
It can be characterized by sensor electrical parameter.
The sensitive material that existing adsorbed sensor is used mainly has CNT (CNTs), transition metal oxide
(TMOs).The adsorbed sensor of CNTs film configurations has the advantages that operating temperature is low., Kyushu University in 2003
Suehiro et al. constructs CNTs sensors using dielectrophoresis method, and prove this method construction sensor CNTs films and
Cohesive between electrode more preferably, and successfully tests NH3、NO2、SO2With the gas such as HF., National Yunlin University of Science and Technology in 2005
Huang et al. obtains the vertical orientated end sensors of CNTs tri- using chemical vapour deposition technique, and completes to N2Survey
Examination, but response recovery time is longer.2006, CNTs was bonded in by Korea University of South Korea Lee et al. using silk screen print method
Interdigital electrode surface structure adsorbed sensor, is realized to NO2The detection of gas, synthesis step is simple.But CNTs De contaminations
Difficulty, response recovery time is long, and sensitivity, nor very high, measurement result is rough, with very big defect.TMOs films
The adsorbed sensor of construction has sensitivity high, the short advantage of response recovery time., Italy Brescia university in 2002
Comini et al. uses thermal evaporation, constructs one-dimensional SnO2Nano material sensor, have detected CO, NO2And alcohol gas.
2003, Pennsylvania State University Varghese et al. used anodizing, constructs TiO2Nano-pipe array thin film sensor,
Test result shows the sensor to N2H under environment2、O2Sensitivity is very high, to CO and NH3There is very strong selectivity.2005
Year, Stony Brook University SUNY Sawicka et al. uses method of electrostatic spinning, constructs WO3Nano-wire array film is sensed
Device, it is to NO2Show very high sensitivity characteristic.But TMOs senor operating temperatures are high, and building-up process is complicated, cost compared with
It is high.
The content of the invention
Based on this, the disclosure discloses a kind of rhenium disulfide nano-chip arrays film adsorbed sensor；
The sensor includes electrode basement and sensitive material；
The sensitive material is the rhenium disulfide nano-chip arrays film being orientated perpendicular to electrode basement.
The disclosure further discloses a kind of rhenium disulfide nano-chip arrays film adsorbed sensor preparation method, methods described
Comprise the following steps：
S100, cleaning electrode substrate, then lead to inert gas and the cell substrate after cleaning are dried；
S200, the first container that will be equipped with sulphur are placed on the upstream portion of quartz ampoule in tube furnace, will be equipped with three oxidations
The second container of rhenium is placed on the downstream part of quartz ampoule, and the second container of rhenium trioxide is placed in the center of tube furnace；
Electrode basement is positioned over to the second container upper end equipped with rhenium trioxide down；
S300, inert gas is passed through into quartz ampoule, to discharge the air in quartz ampoule；
S400, using heating tape the first container equipped with sulphur is heated, heating-up temperature rises in 20~30min
250~350 DEG C, the temperature is then kept to first 30~40min of container continuous heating equipped with sulphur；
The second container equipped with rhenium trioxide is heated using tube furnace, heating-up temperature rises to about in 20~30min
650~750 DEG C, the temperature is then kept to 30~40min of second container continuous heating equipped with rhenium trioxide；
Simultaneously under atmospheric pressure, continue to be passed through inert gas into quartz ampoule；
S500, after the heat time of setting to be achieved, stop the work of heating tape and tube furnace, reaction unit is naturally cold
But to after room temperature, taking out the electrode basement surface sensor covered with sensitive material.
The disclosure has following technique effect：
1st, the sensor construction described in the disclosure is simple, small volume, prepares that cost is low, synthesis is simple, particularly nanometer sheet
It is vertical orientated, the sensor is compared to existing sensor, also with sensitivity is high, response recovery time is short, accuracy is good
Advantage.
2nd, the disclosure is constituted by making rhenium disulfide nano-chip arrays film uniform vertical be grown in electrode basement surface
Adsorbed sensor, it is possible to achieve to gas, temperature, humidity detection.The sensor is based on CNT and mistake with existing
Metal oxide materials, the sensor parallel to electrode basement superficial growth are crossed to compare, due to rhenium disulfide nanometer sheet perpendicular to
Electrode basement superficial growth, it is possible to adsorb more gas molecules, sensitivity is higher；Its vertical stratification also helps gas
The diffusion of molecule so that response recovery time is shorter.The disclosure is made the sensor and added using chemical vapour deposition technique
Work, preparation cost is low, synthesis is simple.
Brief description of the drawings
Fig. 1 is a kind of vertical orientated rhenium disulfide nano-chip arrays film absorption type sensing in disclosure one embodiment
The structural representation of device；
Wherein：1st, golden interdigital electrode；2nd, ceramic insulation sheet substrate；3rd, the nanometer sheet material on sensitive gas region is thin
Film；
Fig. 2 is a kind of vertical orientated rhenium disulfide nano-chip arrays film absorption type sensing in disclosure one embodiment
Device utilizes the schematic diagram that chemical vapour deposition technique (CVD) is synthesized；
Wherein：1st, quartz ampoule (is divided into upstream portion a and downstream part b)；2nd, heating tape；3rd, the evaporating dish of sulphur is filled；
4th, tube furnace；5th, the evaporating dish of rhenium trioxide is filled；6th, electrode basement；7th, the two vertical orientated sulphur of electrode basement Surface Creation
Change rhenium film；
Fig. 3 is vertical orientated rhenium disulfide nano-chip arrays film adsorbed sensor in disclosure one embodiment
Learn the reaction condition of vapour deposition process (CVD) synthesis；
Wherein：The curve of lower section represents the heating condition of sulphur in figure；The curve of top represents adding for rhenium trioxide in figure
Heating curve；
Fig. 4 is that vertical orientated rhenium disulfide nano-chip arrays film adsorbed sensor in disclosure one embodiment adds
The SEM photograph of sensor after the completion of work；
Wherein：A-quadrant represents equally distributed rhenium disulfide nanometer sheet on gold electrode；Between the adjacent interdigital finger of B region representations
Gap in equally distributed rhenium disulfide nanometer sheet；
Fig. 5 is that vertical orientated rhenium disulfide nano-chip arrays film adsorbed sensor in disclosure one embodiment adds
The dynamic response curve that sensor resistance changes with humidity after the completion of work；
Wherein：RH represents humidity；Test at room temperature, the curve with interval square pattern represents that humidity is 30%
When, sensor resistance dynamic response curve；Curve with spaced-apart circular pattern represent humidity be 40% when, sensor resistance move
State response curve；With interval triangle pattern curve represent humidity be 50% when, sensor resistance dynamic response curve.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described further to the disclosure.
In one embodiment, a kind of rhenium disulfide nano-chip arrays film adsorbed sensor,
The sensor includes electrode basement and sensitive material；
The sensitive material is the rhenium disulfide nano-chip arrays film being orientated perpendicular to electrode basement.
In the present embodiment by making rhenium disulfide nano-chip arrays film uniform vertical be grown in electrode basement surface structure
Into adsorbed sensor, it is possible to achieve to gas, temperature, humidity detection.The sensor is based on CNT with existing
Compared with transition metal oxide material, parallel to the sensor of electrode basement superficial growth, because rhenium disulfide nanometer sheet is hung down
Directly in electrode basement superficial growth, it is possible to adsorb more gas molecules, sensitivity is higher；Its vertical stratification is also helped
The diffusion of gas molecule so that response recovery time is shorter.
In one embodiment, the electrode basement includes gold electrode and dielectric substrate thin slice；
The gold electrode is attached on dielectric substrate thin slice, constitutes interdigital electrode；
The rhenium disulfide nano-chip arrays film is used to realize the electrical connection between interdigital electrode.
More excellent, the gold electrode is attached on dielectric substrate thin slice, is constituted interdigital electrode and is specifically included：The gold electrode
It is attached to using electron beam plated film photoetching process on dielectric substrate thin slice, two pieces of gold electrodes intersect in comb shape and do not connect but
Touch, constitute interdigital electrode.
Further, the intersection region of the interdigital electrode is located at the center of sensor, for adsorbing sensitive gas；
The cross sectional area of the interdigital electrode is determined by the width and gap of interdigital electrode, is 1~2mm2。
In the present embodiment, different inter-digital electrode widths causes cross sectional area different with clearance distance, sensor
Initial resistance is determined that sensor accuracy in detection and initial resistivity value have relation by cross sectional area.The sensitive gas bag
Water, alcohol vapour etc. are included, the sensitive gas can make changing for the resistance value of sensor, so as to obtain sensor to certain
Plant the response of sensitive gas.
In one embodiment, the logarithm of interdigital electrode is 1-30 pairs in the sensor；
The width of the single interdigital electrode is 1~20um, and the Interdigital Space distance of adjacent inter-digital electrodes is 1~20um；
The gold electrode thickness is 1~100nm.
More excellent, the width of single interdigital electrode is about 20um, and the clearance distance between adjacent interdigital finger is about 10um, interdigital
Electrode logarithm is 20 pairs, and gold electrode thickness is about 50nm.
In the present embodiment, the effect of the interdigital electrode is：, can be with so that the equivalent resistance of sensitive material is parallel with one another
Reduce initial resistance.Interdigital electrode logarithm is more, more equivalent to parallel branch, and initial resistance also just drops more, and initial
Resistance is smaller, and influence of the extraneous factor such as temperature to sensor is also just smaller, and measurement accuracy is improved, and performance gets a promotion.
Interdigital electrode logarithm typically takes more than 20.
In one embodiment, the dielectric substrate thin slice is made up of ceramic insulating material or silicon chip.
In the present embodiment, metallization performance can be improved using silicon chip dielectric substrate thin slice, mechanicalness is also preferable.
In one embodiment, the rhenium disulfide nano-chip arrays film normal grows in electrode basement, two sulphur
Change rhenium nanometer sheet, which is evenly distributed in electrode basement, constitutes conductive film, realizes the electrical connection between interdigital electrode.
More excellent, a width of 1~50um of rhenium disulfide nanometer sheet length, thickness is about 1~100nm.
In the present embodiment, the rhenium disulfide nano-chip arrays film normal grows in electrode basement, beneficial to sensor
Adsorb more sensitive gas.A width of 1~the 50um of rhenium disulfide nanometer sheet length, thickness is about 1~100nm, and rhenium disulfide is received
Rice piece length and width are bigger, and the connectivity between nanometer sheet is better, so that it is guaranteed that the electrical connection of material.Nanometer sheet is thinner, specific surface area
Bigger, the gas molecule of absorption is more, and De contamination is simple, the sensitivity of sensor is higher, response speed also faster.
In one embodiment, a kind of rhenium disulfide nano-chip arrays film adsorbed sensor preparation method, the side
Method comprises the following steps：
It the described method comprises the following steps：
S100, cleaning electrode substrate, then lead to inert gas and the cell substrate after cleaning are dried；
S200, the first container that will be equipped with sulphur are placed on the upstream portion of quartz ampoule in tube furnace, will be equipped with three oxidations
The second container of rhenium is placed on the downstream part of quartz ampoule, and the second container of rhenium trioxide is placed in the center of tube furnace；
Electrode basement is positioned over to the second container upper end equipped with rhenium trioxide down；
S300, inert gas is passed through into quartz ampoule, to discharge the air in quartz ampoule；
S400, using heating tape the first container equipped with sulphur is heated, heating-up temperature rises in 20~30min
250~350 DEG C, the temperature is then kept to first 30~40min of container continuous heating equipped with sulphur；
The second container equipped with rhenium trioxide is heated using tube furnace, heating-up temperature rises to about in 20~30min
650~750 DEG C, the temperature is then kept to 30~40min of second container continuous heating equipped with rhenium trioxide；
Simultaneously under atmospheric pressure, continue to be passed through inert gas into quartz ampoule；
S500, after the heat time of setting to be achieved, stop the work of heating tape and tube furnace, reaction unit is naturally cold
But to after room temperature, taking out the electrode basement surface sensor covered with sensitive material.
It is more excellent, using acetone, methanol and isopropanol successively cleaning electrode substrate or utilize third in the step S100
Ketone, ethanol and deionized water cleaning electrode substrate successively；
The first container and second container in the step S200 include alumina evaporation ware or high quartz crucible.
In one embodiment, as shown in figure 1, the vertical orientated rhenium disulfide nano-chip arrays film absorption type sensing
Device, including electrode basement and sensitive material two parts.Electrode basement is made up of gold electrode and dielectric substrate, utilizes electron beam plated film
Gold thin film is attached in ceramic insulation sheet substrate by technique, recycles ultraviolet photolithographic technique in gold thin film table surface forming electrode figure
Case, finally under the protection of photoresist, corrosion gold thin film obtains electrode basement in corrosive liquid.Two pieces of gold electrodes constitute interdigital electricity
Pole shape, the width of single interdigital electrode is about 20um, and the clearance distance between adjacent interdigital finger is about 10um, interdigital electrode logarithm
For 20 pairs, gold electrode thickness is about 50nm.Sensitive material is the rhenium disulfide nanometer sheet battle array perpendicular to electrode basement superficial growth
Row film, a width of 1um~20um of nanometer sheet length, thickness is about 10nm, and the region area of sensitive gas is about 1.2mm2。
More excellent, in another embodiment：The dielectric substrate can use silicon sheet material, improve metallization performance,
Mechanicalness is also preferable.
More excellent, in another embodiment：When interdigital electrode clearance distance is constant, it is considered to increase interdigital electrode logarithm
To 40 pairs, the region area of sensitive gas increases to about 5mm2。
Using chemical vapour deposition technique (CVD), with reference to Fig. 2 and Fig. 3, vertical orientated rhenium disulfide nano-chip arrays are synthesized
The scheme of film is as follows：
(1) using acetone and methanol, isopropanol successively thoroughly cleaning electrode basement, then lead to nitrogen and carry out drying；
(2) reaction unit carries one a diameter of 1 inch of quartzy transverse tube, and one is equipped with 250mg sulphur (purity ＞
99.9%) alumina evaporation ware is placed on the upstream portion of quartz ampoule, and another is equipped with 1mg rhenium trioxides (purity ＞
99.9%) alumina evaporation ware is placed on the downstream part of quartz ampoule, is placed in the center of tube furnace.Electrode basement is placed down
In equipped with ReO3Evaporating dish upper end；
(3) open air pump and nitrogen is passed through into quartz ampoule, to discharge air therein；
(4) bring the evaporating dish equipped with sulphur using heating to heat, set temperature to rise to 260 DEG C in 25min, then
Keep 260 DEG C of continuous heating 35min.Meanwhile, given using tube furnace and ReO is housed3Evaporating dish heating, set temperature in 25min
720 DEG C are inside risen to, 720 DEG C, continuous heating 35min are then kept.Under atmospheric pressure, continue with 20sccm speed to stone
Ying Guanzhong is passed through argon gas；
(5) after the heat time for reaching setting, the work of heating tape and tube furnace is stopped, question response device is naturally cooled to
After room temperature, the surface electrode basement covered with sensitive material is taken out.
The sensor SEM photograph obtained using CVD is given in Fig. 4, it can be seen that rhenium disulfide nanometer sheet is in golden electricity
Pole A, interdigital electrode gap B and AB boundaries are all that uniform vertical grows in electrode basement, it is ensured that the absorption type is sensed
The reliability of device electrical connection.
More excellent, in another embodiment：The CVD preparation methods can be changed by way of changing synthesis material proportioning
Enter.Control S and ReO3The amount of raw material, for example, keep S content 250mg constant, increases the content of rhenium disulfide to 2mg, to change
Become growing state of the rhenium disulfide on electrode basement surface, it is thin to obtain the different rhenium disulfide nano-chip arrays of pattern, structure
Film.
More excellent, in another embodiment：The CVD preparation methods can be improved by way of changing synthesis strategy.
The heating-up temperature and heat time of heating tape and tube furnace to two evaporating dishes are controlled, to change rhenium disulfide in electrode basement
The growing state on surface, to obtain the rhenium disulfide nano-chip arrays film that pattern, structure are different.
The sensor is carried out using sensor detector to give sensor resistance with humidity in experimental test, Fig. 5
The dynamic response curve of change.As rhenium disulfide nanometer sheet adsorption H2After O molecules, H2O can discharge electronics to rhenium disulfide,
And rhenium disulfide is N-type semiconductor, majority carrier is electronics.So, it is compound equivalent to occurring with hole when it obtains electronics
Electron amount reduce, for conductive free electron quantity increase, depleted of electrons layer narrows.Macro manifestations increase for electrical conductivity
Plus, resistance value is reduced.It is additionally, since rhenium disulfide nanometer sheet to grow perpendicular to electrode basement, more H can be adsorbed2O points
Son, should significantly increase sensitivity, reduce response recovery time in theory.By can also be, it is evident that being passed through during 20s in figure
Vapor, the response time is about 20s or so.Stop water flowing steam during 80s, start to be passed through drying nitrogen, recovery time is about 15s
Left and right.Moreover, resistance of sensor is significantly increased with the increase of humidity, sensitivity is 10 orders of magnitude, experimental result and before
Principle analysis be consistent.
More excellent, in another embodiment：If the sensor is used for environmental monitoring, tested gas can also be
CO、C2H2、O3、NO2、NH3、SO2Deng pernicious gas.Widely should very much moreover, can also have in electrical equipment online monitoring field
With.
Specific embodiment principle of this disclosure is applied in the disclosure and embodiment is set forth, is implemented to more than
The explanation of example, is only intended to help the application method for understanding the disclosure and its core concept.The disclosure in embodiment and
It will change according to actual conditions in application, above-described embodiment is not used to limit the disclosure.This is not being departed from
In the case of technical characteristic given by public technology scheme, increase, the deformation or same with this area made to technical characteristic
The replacement of content, all should belong to the protection domain of the disclosure.
Claims (10)
1. a kind of rhenium disulfide nano-chip arrays film adsorbed sensor, it is characterised in that：
The sensor includes electrode basement and sensitive material；
The sensitive material is the rhenium disulfide nano-chip arrays film being orientated perpendicular to electrode basement.
2. sensor according to claim 1, it is characterised in that preferred, the electrode basement includes gold electrode and exhausted
Edge backing sheet；
The gold electrode is attached on dielectric substrate thin slice, constitutes interdigital electrode.
3. sensor according to claim 2, it is characterised in that：The gold electrode is attached on dielectric substrate thin slice, structure
Specifically included into interdigital electrode：The gold electrode is attached on dielectric substrate thin slice using electron beam plated film photoetching process, two pieces
Gold electrode intersects in comb shape and not contacted but, constitutes interdigital electrode.
4. sensor according to claim 3, it is characterised in that：The intersection region of the interdigital electrode is located at sensor
Center, for adsorbing sensitive gas；
The cross sectional area of the interdigital electrode by interdigital electrode width and constitute two pieces of gold electrodes of the interdigital electrode
Gap determined.
5. sensor according to claim 3, it is characterised in that：The logarithm of interdigital electrode is 1~30 in the sensor
It is right；
The width of the single interdigital electrode is 1~20um, and the Interdigital Space distance of adjacent inter-digital electrodes is 1~20um；
The gold electrode thickness is 1~100nm.
6. sensor according to claim 2, it is characterised in that：The dielectric substrate thin slice is by ceramic insulating material or silicon
Piece is made.
7. sensor according to claim 2, it is characterised in that：The rhenium disulfide nano-chip arrays film normal is in electricity
Pole substrate grown, the rhenium disulfide nanometer sheet, which is evenly distributed in electrode basement, constitutes conductive film, realizes between interdigital electrode
Electrical connection.
8. sensor according to claim 7, it is characterised in that：A length of 1~the 50um of rhenium disulfide nanometer sheet, it is a width of
1~50um, thickness is 1~100nm.
9. a kind of rhenium disulfide nano-chip arrays film adsorbed sensor preparation method, it is characterised in that：Methods described includes
Following steps：
S100, cleaning electrode substrate, then lead to inert gas and the cell substrate after cleaning are dried；
S200, the first container that will be equipped with sulphur are placed on the upstream portion of quartz ampoule in tube furnace, will be equipped with rhenium trioxide
Second container is placed on the downstream part of quartz ampoule, and the second container of rhenium trioxide is placed in the center of tube furnace；
Electrode basement is positioned over to the second container upper end equipped with rhenium trioxide down；
S300, inert gas is passed through into quartz ampoule, to discharge the air in quartz ampoule；
S400, using heating tape the first container equipped with sulphur being heated, heating-up temperature rises to 250 in 20~30min~
350 DEG C, the temperature is then kept to first 30~40min of container continuous heating equipped with sulphur；
The second container equipped with rhenium trioxide is heated using tube furnace, heating-up temperature rises to about 650 in 20~30min~
750 DEG C, the temperature is then kept to 30~40min of second container continuous heating equipped with rhenium trioxide；
Simultaneously under atmospheric pressure, continue to be passed through inert gas into quartz ampoule；
S500, after the heat time of setting to be achieved, stop the work of heating tape and tube furnace, reaction unit is naturally cooled to
After room temperature, the electrode basement surface sensor covered with sensitive material is taken out.
10. method according to claim 9, it is characterised in that：Acetone, methanol and isopropanol are utilized in the step S100
Cleaning electrode substrate or utilize acetone, ethanol and deionized water successively cleaning electrode substrate successively；
The first container and second container in the step S200 include：Alumina evaporation ware, high quartz crucible.
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| CN108002445A (en) * | 2017-12-08 | 2018-05-08 | 温州大学 | The preparation of sulfuration rhenium and cadmium sulfide/sulfuration rhenium composite material |
| CN108862397A (en) * | 2018-06-15 | 2018-11-23 | 肇庆市华师大光电产业研究院 | A kind of method directly growing uniform two selenizings rhenium nanometer sheet on basal electrode and modified electrode and application |
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| CN110467358A (en) * | 2019-07-09 | 2019-11-19 | 广东工业大学 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
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| CN113109401A (en) * | 2021-03-26 | 2021-07-13 | 华南师范大学 | Rhenium disulfide gas sensor and preparation method and application thereof |
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