CN108362741A - A kind of preparation method and its application method of the gas sensor based on metal phthalocyanine - Google Patents
A kind of preparation method and its application method of the gas sensor based on metal phthalocyanine Download PDFInfo
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- CN108362741A CN108362741A CN201810162282.3A CN201810162282A CN108362741A CN 108362741 A CN108362741 A CN 108362741A CN 201810162282 A CN201810162282 A CN 201810162282A CN 108362741 A CN108362741 A CN 108362741A
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- metal phthalocyanine
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The present invention provides a kind of preparation method and its application method of the gas sensor based on metal phthalocyanine, metal phthalocyanine is dissolved in N by the preparation method, in the mixed solution of N dimethylformamides and water, it drips on electrode, the Metal phthalocyanine film being covered on electrode is formed after drying, the electrode is interdigital electrode.The present invention also provides a kind of application methods of the gas sensor based on metal phthalocyanine, sensor is placed in airtight cavity by the application method, in the detection gas for being filled with preset concentration in the airtight cavity and maintain preset concentration atmosphere, then in being filled with dry air or nitrogen in the airtight cavity when recovery, and use laser irradiation sensor, detection gas are made to be desorbed, this method can effectively solve the problems, such as that metal phthalocyanine gas sensor in the prior art response and resume speed are slow and can not room temperature detection.
Description
Technical field
The invention belongs to field of gas detection, and in particular to a kind of preparation method and its application method of gas sensor.
Background technology
Currently, commercial gas sensor is mainly with INVENTIONConventional metal-oxide semiconductor transducer and solid-state electrolyte sensor
Based on, to gas detection concentration in 100 a ten thousandths (Part Per Million, ppm) magnitude, and exists and such as need
It works at relatively high temperatures, consumes the problems such as power is big, and sensitivity is low, poor anti jamming capability.
Metal phthalocyanine (Metal Phthalocyanine, MPc) has unique big ring conjugated structure, is that a kind of performance is excellent
Different organic semiconducting materials, therefore organic gas sensor can be prepared as sensitive material.Compared to conventional metals oxygen
Compound semiconductor transducer and solid-state electrolyte sensor, MPc gas sensors are abundant, at low cost with raw material sources, are film-made
Simple for process, the advantages that being easy to other technical compatibilities.What is more important, MPc molecules have structure Scalability, can be right
Central metal, conjugate planes electron cloud and peripheric substitution base in MPc molecules carry out controllable adjustment, to be MPc points of realization
Son there is higher detection sensitivity and good selectivity to provide possibility specific gas molecule at room temperature.
However, compared to the gas sensor of metal semiconductor type, the response of metal phthalocyanine and recovery time are longer, even
Position can not be returned to, this just gives its business application band prodigious problem.In addition, the gas sensing based on metal phthalocyanine
Device, which is also required to suitably heat, can just show more excellent response performance, this brings no small difficulty to the making of sensor.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of gases based on metal phthalocyanine
The preparation method and its application method of sensor, for solving metal phthalocyanine gas sensor response in the prior art and restoring
Speed is slow, can not room temperature detection the problem of.
In order to achieve the above objects and other related objects, the present invention provides a kind of gas sensor based on metal phthalocyanine
Preparation method：Metal phthalocyanine is dissolved in n,N-Dimethylformamide (DMF) and the mixed solution of water, drop is done in electrode surface
The Metal phthalocyanine film being covered on electrode is formed after dry；The electrode is interdigital electrode.
Preferably, the average film thickness of the Metal phthalocyanine film is 50~500nm, and the Metal phthalocyanine film is by Nanowire
The average length of dimension composition, the nanofiber is 50~500nm.
Preferably, the mass ratio of the DMF and water is 0.1~10:1.
Preferably, the preparation of the metal phthalocyanine includes the following steps：
Step 1：By trimellitic anhydride, urea, divalent metal chloride and ammonium molybdate mixed grinding at powder after, will
Powder after the grinding is added in container, is heated to 180~250 DEG C, is kept for 6~24 hours；
Step 2：After the product obtained in step 1 is impregnated 12~24 hours with the hydrochloric acid solution of 0.5~2mol/L, mistake
Filter, washing make the pH value of product reach 6~8；
Step 3：The product obtained in step 2 is transferred in container, with a concentration of 0.5~2mol/L sodium hydroxide solutions
It boils 20~120 minutes, filtering or centrifugation obtain solid product；
Step 4：The solid product that obtains in step 3 is transferred in container, the hydrogen-oxygen containing 0.5~2mol/L is added
Change the saturated nacl aqueous solution of sodium, flows back 6~12 hours at a temperature of 80~100 DEG C；
Step 5：After solution cooling, solution is added in distilled water, then by filtering or centrifuging removal insoluble matter；
Step 6：Hydrochloric acid is added dropwise to the solution obtained in step 5, after pH is adjusted to 3 hereinafter, standing 8~48 hours, filtering
Go out the sediment in solution, using methanol and distillation water washing, is finally dried to obtain metal phthalocyanine.
Preferably, the divalent metal chloride is CuCl2、FeCl2、NiCl2、CoCl2Or ZnCl2。
Preferably, the metal phthalocyanine is tetracarboxylic acid metal phthalocyanines, and general formula is MPc (COOH)4, M therein be Cu,
Fe, Ni, Co or Zn.
Preferably, the mixing molar ratio of the trimellitic anhydride, urea, divalent metal chloride and ammonium molybdate is：
400：2000~4000：100~200：1~5.
The present invention also provides a kind of application methods of the gas sensor based on metal phthalocyanine, include the following steps
Step 1：The gas sensor based on metal phthalocyanine is placed in airtight cavity, dry air or nitrogen are filled with
Gas, and voltage is applied to the gas sensor based on metal phthalocyanine；
Step 2：It is filled with the detection gas of preset concentration in the airtight cavity and maintains preset concentration atmosphere；
Step 3：Dry air or nitrogen are filled in the airtight cavity, and using laser irradiation based on metal phthalocyanine
Gas sensor makes detection gas be desorbed.
Preferably, the detection gas are NO2、NO、SO2、Cl2Or O3One or more of mixed gas.
Preferably, the optical maser wavelength is 390~500nm, and the power of laser is 10~500mW.
Preferably, the laser irradiation incidence angle is 0~60 °, and laser irradiation distance is 0~30cm.
As described above, preparation method and its use of a kind of gas sensor based on metal phthalocyanine provided by the invention
Method has the following advantages：
1) the present invention provides a kind of simple film-forming process, metal phthalocyanine is dissolved in the mixed solution of DMF and water, then
It being added drop-wise on electrode, film forming is uniform, and phthalocyanine can be crystallized effectively as nanofiber, formed conductive network, accelerated electronics conduction,
Improve air-sensitive response speed.
2) the present invention provides a kind of preparation methods of metal phthalocyanine, compared to past phthalocyanine synthetic method, this method
Synthesis step is simple, and aggregate velocity is fast, high yield rate.
3) the present invention provides a kind of application methods of gas sensor, have used laser irradiation auxiliary to restore, have made metal
The resume speed of phthalocyanine gas sensor is significantly increased.
4) the metal phthalocyanine air-sensitive detection limit provided by the invention is low, and selectivity is good.
The technique effect of the design of the present invention, specific technical solution and generation is made into one below with reference to preferred embodiment
Step explanation, to fully understand the purposes, features and effects of the present invention.
Description of the drawings
Fig. 1 is the scanning electron microscope test figure of the metal phthalocyanine of the synthesis of the preferred embodiment of the present invention；
Fig. 2 is that the scanning electron microscope in interdigital electrode is added dropwise in the metal phthalocyanine of the preferred embodiment of the present invention
Test chart；
Fig. 3 is that the sensor of the preferred embodiment of the present invention is placed in the NO of a concentration of 50ppm2The gas measured in gas
Quick response diagram；
Fig. 4 is that the sensor of the preferred embodiment of the present invention is placed in the NO of a concentration of 50ppb-50ppm2It is surveyed in gas
The air-sensitive response diagram obtained；
Fig. 5 is that the sensor of the preferred embodiment of the present invention is placed in the air-sensitive measured in the atmosphere of a variety of gas with various
Test chart.
Specific implementation mode
Multiple preferred embodiments that the present invention is introduced below with reference to Figure of description, keep its technology contents more clear and just
In understanding.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention not only limits
The embodiment that Yu Wenzhong is mentioned.
Embodiment 1：
The present embodiment provides a kind of preparation methods of the gas sensor based on metal phthalocyanine：Metal phthalocyanine is dissolved in DMF
In the mixed solution of water, the mass ratio of DMF and water is 1:1, it is thin to form the metal phthalocyanine being covered on electrode on electrode for drop
The average film thickness of film, film is 200nm；The Metal phthalocyanine film is made of nanofiber, the average length of the nanofiber
Degree is 200nm；The electrode is interdigital electrode.
The preparation of the metal phthalocyanine includes the following steps：
Step 1：By trimellitic anhydride, urea, CoCl2And ammonium molybdate is according to molar ratio 400:2500:150:1 mixing
It pulverizes last, the powder after the grinding is added in container, be heated to 200 DEG C, kept for 12 hours；
Step 2：After the product obtained in step 1 1mol/L salt acid soak 14 hours, it is filtered, washed the pH for making product
Value reaches 7；
Step 3：The product obtained in step 2 is transferred in container, is boiled with a concentration of 1mol/L sodium hydroxide solutions
60 minutes, solid product is obtained by filtration；
Step 4：The solid product that obtains in step 3 is transferred in container, is added containing 1mol/L sodium hydroxides
Saturated nacl aqueous solution flows back 8 hours at a temperature of 100 DEG C；
Step 5：After solution cooling, solution is added in distilled water, then be removed by filtration insoluble matter；
Step 6：Hydrochloric acid is added dropwise to the solution obtained in step 5, pH is adjusted to 2, after standing 14 hours, is filtered out in solution
Sediment, using methanol and distillation water washing, be finally dried to obtain tetracarboxylic cobalt phthalocyanine CoPc (COOH)4。
Fig. 1 is the scanning electron microscope test figure of the metal phthalocyanine synthesized in the present embodiment；Fig. 2 is golden in the present embodiment
Belong to phthalocyanine and the scanning electron microscope test figure in interdigital electrode is added dropwise.As can be seen from the figure the metal phthalocyanine of the present embodiment
Preparation method film forming is uniform, and the good crystallinity in the mixed solution of DMF and water easily forms conductive network.
Embodiment 2
According to embodiment 1, this implementation provides a kind of application method of the gas sensor based on metal phthalocyanine, including following
Step：
Step 1：Sensor is placed in airtight cavity, is filled with dry air, and 0.5V voltages are applied to sensor；
Step 2：In the NO for being passed through 50ppm in the airtight cavity2Gas simultaneously maintains the concentration gases atmosphere；
Step 3：In being filled with dry air in the airtight cavity, and the use of wavelength is the laser that 395nm power is 50mW
Sensor is irradiated, NO is made2Desorption, the laser irradiation incidence angle are 0 °, and laser irradiation distance is 10cm.
Fig. 3 is the NO that sensor is placed in a concentration of 50ppm in the present embodiment2The air-sensitive response diagram measured in gas restores
Part uses laser irradiation auxiliary.Wherein Ig is the current value being passed through after test gas, and Ia is electricity when being passed through dry air
Flow valuve；Fig. 4 is the NO that sensor is placed in a concentration of 50ppb-50ppm in the present embodiment2The air-sensitive response diagram measured in gas；Figure
5 be that sensor is placed in the air-sensitive test chart measured in the atmosphere of a variety of gas with various in the present embodiment.It can be seen from the figure that base
In the gas sensor NO of the metal phthalocyanine2Response sensitivity is high, and resume speed is fast under laser irradiation auxiliary, and with compared with
Low response limit and excellent selectivity.
Embodiment 3
The present embodiment provides a kind of preparation methods of the gas sensor based on metal phthalocyanine：Metal phthalocyanine is dissolved in DMF
In the mixed solution of water, the mass ratio of DMF and water is 2:1, it is thin to form the metal phthalocyanine being covered on electrode on electrode for drop
The average film thickness of film, film is 100nm；The Metal phthalocyanine film is made of nanofiber, the average length of the nanofiber
Degree is 100nm；The electrode is interdigital electrode.
The preparation of metal phthalocyanine includes the following steps：
Step 1：By trimellitic anhydride, urea, NiCl2And ammonium molybdate is according to molar ratio 400:3000:180:4 mixing
It pulverizes last, the powder after the grinding is added in container, be heated to 220 DEG C, kept for 18 hours；
Step 2：After the product obtained in step 1 1.5mol/L salt acid soak 18 hours, being filtered, washed makes product
PH value reaches 7.5；
Step 3：The product obtained in step 2 is transferred in container, is boiled with a concentration of 1.5mol/L sodium hydroxide solutions
Boiling 40 minutes, centrifugation obtain solid product；
Step 4：The solid product that obtains in step 3 is transferred in container, is added containing 1.5mol/L sodium hydroxides
Saturated nacl aqueous solution, flow back 10 hours at a temperature of 95 DEG C；
Step 5：After solution cooling, solution is added in distilled water, then insoluble matter is removed by centrifugation；
Step 6：Hydrochloric acid is added dropwise to the solution obtained in step 5, pH is adjusted to 1, after standing 18 hours, is filtered out in solution
Sediment, using methanol and distillation water washing, be finally dried to obtain tetracarboxylic nickel phthalocyanine NiPc (COOH)4。
Embodiment 4
According to embodiment 3, this implementation provides a kind of application method of the gas sensor based on metal phthalocyanine, including following
Step：
Step 1：Sensor is placed in airtight cavity, is filled with nitrogen, and 0.5V voltages are applied to sensor；
Step 2：In the NO for being passed through 50ppm in the airtight cavity2Gas simultaneously maintains the concentration gases atmosphere；
Step 3：In being filled with nitrogen in the airtight cavity, and the use of wavelength is the laser irradiation that 450nm power is 100mW
Sensor makes NO2Desorption, the laser irradiation incidence angle are 20 °, and laser irradiation distance is 15cm.
In conclusion the metal phthalocyanine preparation method film forming of the embodiment of the present invention is uniform, in the mixed solution of DMF and water
Good crystallinity easily forms conductive network；Gas sensor NO based on the metal phthalocyanine2Response sensitivity is high, in laser irradiation
The lower resume speed of auxiliary is fast, and has lower response limit and excellent selectivity.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of preparation method of the gas sensor based on metal phthalocyanine, which is characterized in that metal phthalocyanine is dissolved in N, N- bis-
In the mixed solution of methylformamide and water, drop forms the Metal phthalocyanine film being covered on electrode in electrode surface after dry,
The electrode is interdigital electrode.
2. a kind of preparation method of the gas sensor based on metal phthalocyanine as described in claim 1, which is characterized in that described
The mass ratio of N,N-dimethylformamide and water is 0.1~10 in mixed solution:1.
3. a kind of preparation method of the gas sensor based on metal phthalocyanine as described in claim 1, which is characterized in that described
The average film thickness of Metal phthalocyanine film is 50~500nm, and the Metal phthalocyanine film is made of nanofiber, the nanofiber
Average length be 50~500nm.
4. a kind of preparation method of the gas sensor based on metal phthalocyanine as described in claim 1, which is characterized in that described
Metal phthalocyanine is prepared via a method which, is specifically included：
Step 1：Trimellitic anhydride, urea, divalent metal chloride and ammonium molybdate are mixed and pulverize it is last, by institute
It states the powder after grinding to be added in container, is heated to 180~250 DEG C, kept for 6~24 hours；
Step 2：After the product obtained in step 1 is impregnated 12~24 hours with the hydrochloric acid solution of 0.5~2mol/L, filters, washes
Washing makes the pH value of product reach 6~8；
Step 3：The product obtained in step 2 is transferred in container, is boiled with a concentration of 0.5~2mol/L sodium hydroxide solutions
20~120 minutes, filtering or centrifugation obtained solid product；
Step 4：The solid product that obtains in step 3 is transferred in container, is added containing 0.5~2mol/L sodium hydroxides
Saturated nacl aqueous solution flows back 6~12 hours at a temperature of 80~100 DEG C；
Step 5：After solution cooling, solution is added in distilled water, then by filtering or centrifuging removal insoluble matter；
Step 6：Hydrochloric acid is added dropwise into the solution obtained in step 5, after pH is adjusted to 3 hereinafter, standing 8~48 hours, filters out
Sediment in solution is finally dried to obtain metal phthalocyanine using methanol and distillation water washing.
5. a kind of preparation method of the gas sensor based on metal phthalocyanine as claimed in claim 4, which is characterized in that described
Divalent metal chloride is CuCl in step 12、FeCl2、NiCl2、CoCl2Or ZnCl2In any one.
6. a kind of preparation method of the gas sensor based on metal phthalocyanine as described in claim 1, which is characterized in that described
Metal phthalocyanine is tetracarboxylic acid metal phthalocyanines, and general formula is MPc (COOH)4, M therein is arbitrary in Cu, Fe, Ni, Co or Zn
It is a kind of..
7. a kind of preparation method of the gas sensor based on metal phthalocyanine as claimed in claim 4, which is characterized in that described
Trimellitic anhydride, urea, divalent metal chloride and ammonium molybdate mixing molar ratio be：400：2000~4000：100~
200：1~5.
8. a kind of gas biography based on metal phthalocyanine made from a kind of preparation method as described in any one of claim 1-7
The application method of sensor, which is characterized in that include the following steps：
Step 1：The gas sensor based on metal phthalocyanine is placed in airtight cavity, dry air or nitrogen are filled with, and
Voltage is applied to the gas sensor based on metal phthalocyanine；
Step 2：It is filled with the detection gas of preset concentration in the airtight cavity and maintains preset concentration atmosphere；
Step 3：It is filled with dry air or nitrogen in the airtight cavity, and uses gas of the laser irradiation based on metal phthalocyanine
Sensor makes detection gas be desorbed.
9. a kind of application method of the gas sensor based on metal phthalocyanine as claimed in claim 8, which is characterized in that described
Detection gas are NO2、NO、SO2、Cl2Or O3One or more of mixed gas.
10. a kind of application method of the gas sensor based on metal phthalocyanine as claimed in claim 8, which is characterized in that institute
The optical maser wavelength stated is 390~500nm, and the power of laser is 10~500mW, and the laser irradiation incidence angle is 0~60 °,
Laser irradiation distance is 0~30cm.
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| CN109828003A (en) * | 2019-02-18 | 2019-05-31 | 中国石油大学(华东) | It is a kind of based on cadmium sulfide to the inorganic doping method of modifying of the Phthalocyanine semiconductor material containing crown ether |
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| CN113029239A (en) * | 2021-03-11 | 2021-06-25 | 昆山联鲸仪智能科技有限公司 | Multifunctional sensor and preparation method thereof |
| CN113777137A (en) * | 2021-09-24 | 2021-12-10 | 昆明学院 | Gas sensor based on chromium phthalocyanine monomolecular layer film and preparation method and application thereof |
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| CN113777137A (en) * | 2021-09-24 | 2021-12-10 | 昆明学院 | Gas sensor based on chromium phthalocyanine monomolecular layer film and preparation method and application thereof |
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| CN108362741B (en) | 2020-09-08 |
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