CN106770470A - CuPc cuprous oxide composite gas sensor and preparation method thereof - Google Patents
CuPc cuprous oxide composite gas sensor and preparation method thereof Download PDFInfo
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- CN106770470A CN106770470A CN201710006271.1A CN201710006271A CN106770470A CN 106770470 A CN106770470 A CN 106770470A CN 201710006271 A CN201710006271 A CN 201710006271A CN 106770470 A CN106770470 A CN 106770470A
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Abstract
The invention discloses a kind of CuPc cuprous oxide composite gas sensor and preparation method thereof.Gas sensor is to be covered with film-form CuPc cuprous oxide on substrate with electrode, wherein, CuPc is bar-shaped, and cuprous oxide is graininess；Method is first to prepare CuPc sulfuric acid solution, filtered after being added into stirring in deionized water again, obtain filter cake, then, filter cake is first respectively placed in suction filtration after disperseing in bronsted lowry acids and bases bronsted lowry solution, the CuPc for purifying is made to be washed with deionized and dried again, obtain CuPc nanometer rods, afterwards, it is scattered in n-butanol after first mixing CuPc nanometer rods and cuprous oxide nano particle, the mixed solution that will be obtained by autonomous interface dress method again forms CuPc cuprous oxide film in deionized water surface, finally, first film is fished for using the substrate with electrode, the film drying on substrate will be overlying on again, purpose product is obtained.It can be extremely easy to commercially be widely used in the high-sensitivity detection to front three amine gas.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method, especially a kind of CuPc-cuprous oxide (CuPc-Cu2O)
Composite gas sensor and preparation method thereof.
Background technology
As the mankind deepen continuously to strategy of sustainable development understanding, environmental pollution and weather variation issue cause generation
The great attention of various countries of boundary.Trimethylamine is one of main object of national foul gas Environmental capacity, while being also in Fish
The predominant gas produced during breaks down proteins, its content has turned into the important indicator of current aquatic products freshness.Therefore, to front three
The research and development of amine gas high-sensitivity detection material have turned into important research topic, such as Chinese invention patent application CN
A kind of trimethylamine gas sensor that 103063705 A were announced on April 24th, 2013 and preparation method thereof.The patent of invention Shen
Please in the gas sensor that refers to be Al with electrode2O3Air-sensitive film is covered with earthenware, air-sensitive film therein is by SnO2With account for
SnO2The Eu of molal weight 0.5~5%5+Or La5+Composition；Preparation method obtains nano SnO first to use hydro-thermal method2, then adulterate
A certain amount of rare earth element prepares gas sensitive, afterwards, gas sensitive first is coated in into Al2O3The surface of earthenware is made air-sensitive
Electrode tube, then anneal 2~4 hours at being placed on 400~500 DEG C, obtain product.Though this product can be used for trimethylamine
Detection, but all has weak point with its preparation method, and first, the detection sensitivity of product is not high, only 8~10ppm；Its
Secondary, operating temperature during product detection front three amine gas is up to 150~250 DEG C；Finally, preparation method cannot both be accurately controlled
The film thickness of gas sensitive, needs high annealing again, can't obtain the product of trimethylamine detection sensitivity higher.
The content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, there is provided one kind has front three higher
The CuPc of amine gas detection sensitivity-cuprous oxide composite gas sensor.
The invention solves the problems that another technical problem to provide a kind of above-mentioned CuPc-cuprous oxide composite gas sensor
Preparation method.
Be to solve technical problem of the invention, the technical scheme for being used for：CuPc-cuprous oxide composite gas sensor
Including the substrate with electrode, particularly,
Film-form CuPc-cuprous oxide is covered with the substrate with electrode, the film-form CuPc-oxidation is sub-
The thickness of copper is 200~300nm, and it is 1 by weight ratio：3~7 CuPc and cuprous oxide composition；
The CuPc is bar-shaped, a length of 10~15um of its rod, a diameter of 200~300nm of rod；
The cuprous oxide is graininess, and its particle diameter is 80~120nm.
As the further improvement of CuPc-cuprous oxide composite gas sensor：
Preferably, the resistivity of CuPc-cuprous oxide film is 120~160 Ω m.
Preferably, the substrate with electrode is shaped as plane, or curved surface, or tubulose.
Be to solve another technical problem of the invention, another technical scheme for being used for：Above-mentioned CuPc-oxidation
The preparation method of cuprous composite gas sensor includes that autonomous interface dress method, particularly key step are as follows：
, first be placed in CuPc in the sulfuric acid solution of 30~70 DEG C of mass fraction >=95% and stir complete to its by step 1
Dissolving, obtains CuPc sulfuric acid solution, and the volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：8~12 ratio
Example, filters after at least 3h is stirred in the deionized water that CuPc sulfuric acid solution is added 90~100 DEG C, obtains filter cake；
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.08~0.12mol/L and aqueous slkali, is obtained
To the CuPc of purifying, then CuPc to purifying make to be washed with deionized to its filtrate in neutrality after, be placed in 60~100 DEG C
Lower drying, obtains CuPc nanometer rods；
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：3~7 ratio, by two
It is scattered in n-butanol after person's mixing, obtains the mixed solution of 0.005~0.015g/mL, then will be mixed by autonomous interface dress method
Close solution and form CuPc-cuprous oxide film in deionized water surface；
Step 4, at least 5min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode, is obtained
Be overlying on the CuPc-cuprous oxide film on substrate, then the CuPc-cuprous oxide film that will be overlying on substrate be placed in 100~
At least 5min is dried at 140 DEG C, CuPc-cuprous oxide composite gas sensor is obtained.
As the further improvement of the preparation method of CuPc-cuprous oxide composite gas sensor：
Preferably, before mixing with CuPc nanometer rods, at cuprous oxide nano particle is placed in into 100~150 DEG C at least
10h。
Preferably, acid solution is hydrochloric acid solution, or sulfuric acid solution, or salpeter solution.
Preferably, aqueous slkali is sodium hydroxide solution, or potassium hydroxide solution, or lithium hydroxide solution.
Preferably, the substrate with electrode is shaped as plane, or curved surface, or tubulose.
Beneficial effect relative to prior art is：
First, being carried out using ESEM, powder x-ray diffraction and resistance meter respectively to obtained purpose product
Characterize, from its result, purpose product is the film being overlying on the substrate with electrode；Wherein, the thickness of film be 200~
300nm, it is made up of nanometer rods and nano particle, a length of 10~15um of rod of nanometer rods therein, rod a diameter of 200~
300nm, the particle diameter of nano particle is 80~120nm.Film is 1 by weight ratio：3~7 CuPc and cuprous oxide composition；Its
In CuPc for bar-shaped, cuprous oxide is graininess.The resistivity of film is 120~160 Ω m.It is this by CuPc and
Cuprous oxide is assembled into the purpose product of film-form, both because the good stability of CuPc, operating temperature are low, and because of cuprous oxide
Higher sensitivity and fast response characteristic, due also to CuPc and cuprous oxide are to trimethylamine gas sensitization, and both
Combination and complement each other, more because CuPc and cuprous oxide are nanoscale, and the raising purpose product that is highly advantageous to
Sensitivity to gas detection.
It is multiple under various concentrations through carrying out to front three amine gas second, using obtained purpose product as gas sensor
The test of many batches, as the concentration as little as 50ppb of tested gas trimethylamine, remains to effectively detect it.Purpose is produced
Response speed≤4s, recovery time≤20s of the thing to front three amine gas, operating temperature are 100~130 DEG C, the stabilization of its detection
Property, invertibity and repeatability it is all very good.
Third, preparation method is simple, science, efficiently.Not only it has been obtained with front three amine gas detection sensitivity higher
Purpose product --- CuPc-cuprous oxide composite gas sensor, also makes it have response speed faster and recovery time,
And relatively low operating temperature, more there is film thickness to accurately control, be not required to high annealing --- the characteristics of energy-conservation；So that
Purpose product is extremely easy to commercially be widely used in the high-sensitivity detection to front three amine gas.
Brief description of the drawings
Fig. 1 is one of result for being characterized using ESEM (SEM) to purpose product obtained in preparation method.SEM
Image shows that purpose product is made up of nanometer rods and nano particle.
Fig. 2 is one of result for being characterized using powder x-ray diffraction (XRD) instrument to obtained purpose product.XRD is composed
Figure confirms that purpose product is made up of CuPc and cuprous oxide.
Fig. 3 is the response and front three measured in the front three amine gas that the purpose product shown in Fig. 1 is placed under various concentrations
Amine concentration relationship curve map.The condition of test is：It is 10V that the test voltage at purpose product two ends is constant, operating temperature is 100~
130℃.As seen from Figure 3, purpose product has response well to the trimethylamine in 0.05~50ppm of concentration range.
Fig. 4 is that the purpose product shown in Fig. 1 is placed in the purpose measured in the front three amine gas that concentration is 1~50ppb to produce
Concentration gradient figure of the thing to front three amine gas.Same Fig. 3 of condition of test.As seen from Figure 4, purpose product is to front three amine gas
Detection sensitivity is up to 50ppb.
Fig. 5 is that the purpose product shown in Fig. 1 is placed in into being circulated property test in the front three amine gas that concentration is 2ppm
Result figure.Same Fig. 3 of condition of test.As seen from Figure 5, purpose product is tested trimethylamine stability, invertibity and repetition
Property very it is good.
Specific embodiment
Preferred embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Bought from market first or be voluntarily obtained：
CuPc；
The sulfuric acid solution of mass fraction >=95%；
Deionized water；
As the hydrochloric acid solution of acid solution, sulfuric acid solution and salpeter solution；
As the sodium hydroxide solution of aqueous slkali, potassium hydroxide solution and lithium hydroxide solution；
Cuprous oxide nano particle；
N-butanol；
Substrate with electrode, it is shaped as plane or curved surface or tubulose.
Wherein, before cuprous oxide nano particle is mixed with CuPc nanometer rods, cuprous oxide nano particle is placed in
At least 10h at 100~150 DEG C.
Then,
Embodiment 1
What is prepared concretely comprises the following steps：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution that 30 DEG C of mass fraction is 99% be completely dissolved,
Obtain CuPc sulfuric acid solution.Volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：8 ratio, by CuPc
Filtered after 5h is stirred in the deionized water of 90 DEG C of sulfuric acid solution addition, obtain filter cake.
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.08mol/L and aqueous slkali；Wherein, acid is molten
Liquid is hydrochloric acid solution, and aqueous slkali is sodium hydroxide solution, the CuPc for being purified.Deionization is used to the CuPc for purifying again
After water washing is in neutral to its filtrate, dried at being placed in 60 DEG C, obtain CuPc nanometer rods.
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：3 ratio, incite somebody to action both
It is scattered in n-butanol after mixing, obtains the mixed solution of 0.005g/mL.Method is filled by mixed solution in going by autonomous interface again
Ion water surface forms CuPc-cuprous oxide film.
Step 4,5min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode；Wherein, have
CuPc-the cuprous oxide film for being shaped as plane, obtaining being overlying on substrate of the substrate of electrode.The phthalein on substrate will be overlying on again
Cyanines copper-cuprous oxide film dries 9min at being placed in 100 DEG C, is obtained and is similar to shown in Fig. 1, and such as Fig. 2, Fig. 3, Fig. 4 and Fig. 5
In curve shown in CuPc-cuprous oxide composite gas sensor.
Embodiment 2
What is prepared concretely comprises the following steps：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution that 40 DEG C of mass fraction is 98% be completely dissolved,
Obtain CuPc sulfuric acid solution.Volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：9 ratio, by CuPc
Filtered after 4.5h is stirred in the deionized water of 93 DEG C of sulfuric acid solution addition, obtain filter cake.
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.09mol/L and aqueous slkali；Wherein, acid is molten
Liquid is hydrochloric acid solution, and aqueous slkali is sodium hydroxide solution, the CuPc for being purified.Deionization is used to the CuPc for purifying again
After water washing is in neutral to its filtrate, dried at being placed in 70 DEG C, obtain CuPc nanometer rods.
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：4 ratio, incite somebody to action both
It is scattered in n-butanol after mixing, obtains the mixed solution of 0.008g/mL.Method is filled by mixed solution in going by autonomous interface again
Ion water surface forms CuPc-cuprous oxide film.
Step 4,6min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode；Wherein, have
CuPc-the cuprous oxide film for being shaped as plane, obtaining being overlying on substrate of the substrate of electrode.The phthalein on substrate will be overlying on again
Cyanines copper-cuprous oxide film dries 8min at being placed in 110 DEG C, is obtained and is similar to shown in Fig. 1, and such as Fig. 2, Fig. 3, Fig. 4 and Fig. 5
In curve shown in CuPc-cuprous oxide composite gas sensor.
Embodiment 3
What is prepared concretely comprises the following steps：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution that 50 DEG C of mass fraction is 97% be completely dissolved,
Obtain CuPc sulfuric acid solution.Volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：10 ratio, by phthalocyanine
Filtered after 4h is stirred in the deionized water of 95 DEG C of copper sulfuric acid solution addition, obtain filter cake.
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.1mol/L and aqueous slkali；Wherein, acid is molten
Liquid is hydrochloric acid solution, and aqueous slkali is sodium hydroxide solution, the CuPc for being purified.Deionization is used to the CuPc for purifying again
After water washing is in neutral to its filtrate, dried at being placed in 80 DEG C, obtain CuPc nanometer rods.
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：5 ratio, incite somebody to action both
It is scattered in n-butanol after mixing, obtains the mixed solution of 0.01g/mL.Method is filled by mixed solution in going by autonomous interface again
Ion water surface forms CuPc-cuprous oxide film.
Step 4,7min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode；Wherein, have
CuPc-the cuprous oxide film for being shaped as plane, obtaining being overlying on substrate of the substrate of electrode.The phthalein on substrate will be overlying on again
Cyanines copper-cuprous oxide film dries 7min at being placed in 120 DEG C, is obtained as shown in figure 1, and as in Fig. 2, Fig. 3, Fig. 4 and Fig. 5
CuPc-cuprous oxide composite gas sensor shown in curve.
Embodiment 4
What is prepared concretely comprises the following steps：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution that 60 DEG C of mass fraction is 96% be completely dissolved,
Obtain CuPc sulfuric acid solution.Volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：11 ratio, by phthalocyanine
Filtered after 3.5h is stirred in the deionized water of 98 DEG C of copper sulfuric acid solution addition, obtain filter cake.
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.11mol/L and aqueous slkali；Wherein, acid is molten
Liquid is hydrochloric acid solution, and aqueous slkali is sodium hydroxide solution, the CuPc for being purified.Deionization is used to the CuPc for purifying again
After water washing is in neutral to its filtrate, dried at being placed in 90 DEG C, obtain CuPc nanometer rods.
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：6 ratio, incite somebody to action both
It is scattered in n-butanol after mixing, obtains the mixed solution of 0.013g/mL.Method is filled by mixed solution in going by autonomous interface again
Ion water surface forms CuPc-cuprous oxide film.
Step 4,8min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode；Wherein, have
CuPc-the cuprous oxide film for being shaped as plane, obtaining being overlying on substrate of the substrate of electrode.The phthalein on substrate will be overlying on again
Cyanines copper-cuprous oxide film dries 6min at being placed in 130 DEG C, is obtained and is similar to shown in Fig. 1, and such as Fig. 2, Fig. 3, Fig. 4 and Fig. 5
In curve shown in CuPc-cuprous oxide composite gas sensor.
Embodiment 5
What is prepared concretely comprises the following steps：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution that 70 DEG C of mass fraction is 95% be completely dissolved,
Obtain CuPc sulfuric acid solution.Volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：12 ratio, by phthalocyanine
Filtered after 3h is stirred in the deionized water of 100 DEG C of copper sulfuric acid solution addition, obtain filter cake.
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.12mol/L and aqueous slkali；Wherein, acid is molten
Liquid is hydrochloric acid solution, and aqueous slkali is sodium hydroxide solution, the CuPc for being purified.Deionization is used to the CuPc for purifying again
After water washing is in neutral to its filtrate, dried at being placed in 100 DEG C, obtain CuPc nanometer rods.
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：7 ratio, incite somebody to action both
It is scattered in n-butanol after mixing, obtains the mixed solution of 0.015g/mL.Method is filled by mixed solution in going by autonomous interface again
Ion water surface forms CuPc-cuprous oxide film.
Step 4,9min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode；Wherein, have
CuPc-the cuprous oxide film for being shaped as plane, obtaining being overlying on substrate of the substrate of electrode.The phthalein on substrate will be overlying on again
Cyanines copper-cuprous oxide film dries 5min at being placed in 140 DEG C, is obtained and is similar to shown in Fig. 1, and such as Fig. 2, Fig. 3, Fig. 4 and Fig. 5
In curve shown in CuPc-cuprous oxide composite gas sensor.
Again respectively from the hydrochloric acid solution or sulfuric acid solution or salpeter solution as acid solution, as the hydroxide of aqueous slkali
Sodium solution or potassium hydroxide solution or lithium hydroxide solution, and it is shaped as the lining with electrode of plane or curved surface or tubulose
Bottom, repeats above-described embodiment 1~5, has equally been obtained as or has been similar to shown in Fig. 1, and as in Fig. 2, Fig. 3, Fig. 4 and Fig. 5
CuPc-cuprous oxide composite gas sensor shown in curve.
Obviously, those skilled in the art can be to CuPc of the invention-cuprous oxide composite gas sensor and its system
Preparation Method carries out various changes and modification without departing from the spirit and scope of the present invention.So, if being repaiied to of the invention these
Change and belong within the scope of the claims in the present invention and its equivalent technologies with modification, then the present invention be also intended to comprising these change and
Including modification.
Claims (8)
1. a kind of CuPc-cuprous oxide composite gas sensor, including the substrate with electrode, it is characterised in that：
Film-form CuPc-cuprous oxide is covered with the substrate with electrode, the film-form CuPc-cuprous oxide
Thickness is 200~300nm, and it is 1 by weight ratio：3~7 CuPc and cuprous oxide composition；
The CuPc is bar-shaped, a length of 10~15um of its rod, a diameter of 200~300nm of rod；
The cuprous oxide is graininess, and its particle diameter is 80~120nm.
2. CuPc according to claim 1-cuprous oxide composite gas sensor, it is characterized in that CuPc-cuprous oxide
The resistivity of film is 120~160 Ω m.
3. CuPc according to claim 1-cuprous oxide composite gas sensor, it is characterized in that substrate with electrode
It is shaped as plane, or curved surface, or tubulose.
4. a kind of preparation method of CuPc described in claim 1-cuprous oxide composite gas sensor, including autonomous interface is filled
Method, it is characterised in that key step is as follows：
Step 1, CuPc first is placed in be stirred to it in the sulfuric acid solution of 30~70 DEG C of mass fraction >=95% be completely dissolved,
CuPc sulfuric acid solution is obtained, the volume ratio according still further to CuPc sulfuric acid solution and deionized water is 1：8~12 ratio, by phthalein
Filtered after at least 3h is stirred in the deionized water of 90~100 DEG C of cyanines copper sulfuric acid solution addition, obtain filter cake；
Step 2, filter cake is first respectively placed in suction filtration after disperseing in the acid solution of 0.08~0.12mol/L and aqueous slkali, obtains pure
The CuPc of change, then CuPc to purifying make to be washed with deionized to its filtrate in neutrality after, done at being placed in 60~100 DEG C
It is dry, obtain CuPc nanometer rods；
Step 3, is first 1 according to the weight ratio of CuPc nanometer rods and cuprous oxide nano particle：3~7 ratio, both are mixed
It is scattered in n-butanol after conjunction, obtains the mixed solution of 0.005~0.015g/mL, then will mix molten by autonomous interface dress method
Liquid forms CuPc-cuprous oxide film in deionized water surface；
Step 4, at least 5min is stood after first fishing for CuPc-cuprous oxide film using the substrate with electrode, is overlying on
CuPc-cuprous oxide film on substrate, the then CuPc-cuprous oxide film that will be overlying on substrate is placed in 100~140 DEG C
Lower drying at least 5min, is obtained CuPc-cuprous oxide composite gas sensor.
5. the preparation method of CuPc according to claim 4-cuprous oxide composite gas sensor, it is characterized in that with phthalein
Before the mixing of cyanines copper nanometer rods, at least 10h at cuprous oxide nano particle is placed in into 100~150 DEG C.
6. the preparation method of CuPc according to claim 4-cuprous oxide composite gas sensor, it is characterized in that acid solution
It is hydrochloric acid solution, or sulfuric acid solution, or salpeter solution.
7. the preparation method of CuPc according to claim 4-cuprous oxide composite gas sensor, it is characterized in that aqueous slkali
It is sodium hydroxide solution, or potassium hydroxide solution, or lithium hydroxide solution.
8. the preparation method of CuPc according to claim 4-cuprous oxide composite gas sensor, it is characterized in that with electricity
The substrate of pole is shaped as plane, or curved surface, or tubulose.
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| CN114100687A (en) * | 2021-11-19 | 2022-03-01 | 陕西科技大学 | Lithium/thionyl chloride battery anode catalytic material CoPc/CuPc and preparation method thereof |
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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 |
| CN109828003B (en) * | 2019-02-18 | 2021-07-23 | 中国石油大学(华东) | Inorganic doping modification method for phthalocyanine molecular semiconductor material containing crown ether based on cadmium sulfide |
| CN113683115A (en) * | 2021-09-01 | 2021-11-23 | 深圳市动盈先进材料有限公司 | Preparation method of semiconductor material for 5G signal transmission |
| CN114100687A (en) * | 2021-11-19 | 2022-03-01 | 陕西科技大学 | Lithium/thionyl chloride battery anode catalytic material CoPc/CuPc and preparation method thereof |
| CN114100687B (en) * | 2021-11-19 | 2023-06-20 | 陕西科技大学 | Lithium/thionyl chloride battery anode catalytic material CoPc/CuPc and preparation method thereof |
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