CN106082308A - The Preparation method and use of hierarchy zinc oxide/cupric oxide nano microsphere - Google Patents
The Preparation method and use of hierarchy zinc oxide/cupric oxide nano microsphere Download PDFInfo
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- CN106082308A CN106082308A CN201610458340.8A CN201610458340A CN106082308A CN 106082308 A CN106082308 A CN 106082308A CN 201610458340 A CN201610458340 A CN 201610458340A CN 106082308 A CN106082308 A CN 106082308A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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
- G01N27/043—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a granular material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to the Preparation method and use of a kind of hierarchy zinc oxide/cupric oxide nano microsphere, the method utilizes solution calcination method to prepare hierarchy zinc oxide and cupric oxide nano microsphere, ordered arrangement with ammonium salt with surfactant regulation and control zinc salt with mantoquita, the Large ratio surface of hierarchy, the efficient electron transfer efficiency of pore structure and ordered structure interface are combined, thus improve the air-sensitive performance of material.By measuring H2When S is adsorbed to material surface, the change of material resistance reaches H2The purpose of S sensing;Measuring signal is voltage, curent change in sensing material resistance variations or the circuit that thus causes;Hierarchy zinc oxide/cupric oxide nano the microsphere obtained by the method for the invention is quickly detecting ppb concentration H2S atmosphere has operating temperature low (125 DEG C), highly sensitive, detection limit concentration up to 1.7 × 10‑9, detection limits low feature.
Description
Technical field
The present invention relates to functional material scientific domain and gas sensing materials field, be specifically related to a kind of with hierarchy oxygen
Change the resistance-type sensing material that zinc/copper oxide is composition, become according to zinc oxide/copper oxide sensitive material resistance at the working temperature
The demarcation of change amount, it is achieved to H2S detects.
Background technology
H2S occurs mainly with the processes such as petroleum refining, selexol process, biogas production, is a kind of irritant stink
Severe toxicity dusty gas.It is commonly exposed to H2In S gaseous environment, breathing and neural disease can be caused.China's odor pollution
Thing discharge standard (GB14554-93) regulation residential block air toxic gas safety concentration is 20-100ppb.A small amount of H2S divides
Son can be as detection signal designation halitosis disease, 10ppb concentration H2S just can deteriorate the performance of hydrogen fuel cell, causes application
Catalyst poisoning in hydrocarbon processing production process.Therefore, ppb level H2The detection of S is for environmental conservation, human health and peace
Full production is significant, develops highly sensitive, detection low, the H of fast response time of limit2S sensing material is the most necessary.
Metal-oxide has absorption and catalysis double effect in terms of gas detecting concurrently, belongs to Surface controlled type.At H2S examines
In survey method, metal oxide resistor formula sensing material has simple in construction, the advantage such as easy to make.Metal oxide resistor formula
Sensing material be generally basede on oxidisability or reducibility gas metal oxide surface absorption or desorption time, oxide resistor occur
Change obtains measuring signal.But, such semiconductor sensing materials'use temperature higher (200 DEG C-500 DEG C), therefore develop work
Make the H of temperature low (room temperature to 200 DEG C)2S sensing material has important practical significance.
Summary of the invention
Present invention aim at, for current gas sensitive to H2The inspection sensitivity of S atmosphere is low, detects limit for height, operating temperature
Height, the feature of response time length, it is provided that the Preparation method and use of a kind of hierarchy zinc oxide/cupric oxide nano microsphere, should
Method utilizes solution calcination method to prepare hierarchy zinc oxide and cupric oxide nano microsphere, regulates and controls zinc with ammonium salt with surfactant
Salt and the ordered arrangement of mantoquita, by the Large ratio surface of hierarchy, the efficient electron transfer of pore structure and ordered structure interface
Efficiency combines, thus improves the air-sensitive performance of material.By measuring H2When S is adsorbed to material surface, the change of material resistance reaches
To H2The purpose of S sensing;Measuring signal is voltage, curent change in sensing material resistance variations or the circuit that thus causes;Logical
Cross the hierarchy zinc oxide/cupric oxide nano microsphere of the method for the invention acquisition in quickly detection ppb concentration H2In S atmosphere
There is operating temperature low (125 DEG C), highly sensitive, the detection low feature of limit.
The preparation method of a kind of hierarchy zinc oxide/cupric oxide nano microsphere of the present invention, follow these steps to into
OK:
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer is molten by nonionic surfactant
Solution is in deionized water, and magnetic agitation forms uniform mixed solution, wherein deionized water and non-ionic surface active for 60 minutes
The mol ratio of agent is 25000-35000:1, and in mixed solution, nonionic surfactant concentration is 0.2mmol/L;
B, being zinc nitrate hexahydrate and Copper nitrate hexahydrate by adding nitrate in step a mixed solution, or chlorate is chlorination
Zinc and copper chloride, continue magnetic agitation 30 minutes, forms uniform mixed solution, wherein nitrate or chlorate with in step a
The mol ratio of nonionic surfactant is 20-100:1, and zinc salt is 0-1:1 with the mol ratio of mantoquita, nitrate in mixed solution
Or perchlorate concentration is 9.0mmol/L;
C, it is ammonium nitrate or ammonium chloride by step b mixed solution adds ammonium salt, continues magnetic agitation 40 minutes, formed all
Even mixed solution, wherein ammonium salt is 300-600:1 with the mol ratio of nonionic surfactant in step a, in mixed solution
Ammonium salt concentration is 0.1mol/L;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 1-3mm, keeps the speed that heats up
Rate 1.0K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature, obtains classification after annealing 2 hours
Structure zinc oxide/cupric oxide nano microsphere.
The mass ratio obtaining zinc oxide in hierarchy zinc oxide/cupric oxide nano microsphere and copper oxide in step d is
1:2。
Hierarchy zinc oxide/cupric oxide nano microsphere that described method obtains is in quickly detection ppb concentration H2In S atmosphere
Purposes.
The Preparation method and use of hierarchy zinc oxide/cupric oxide nano microsphere of the present invention, the method utilizes
Solution calcination method prepares hierarchy zinc oxide/cupric oxide nano microsphere, and uses it for ppb concentration H2The quick inspection of S atmosphere
Survey.The method utilizes ammonium salt and surfactant regulation and control zinc salt and mantoquita ordered arrangement in the solution, adjusts in solution is calcined
Control different annealing temperatures and annealing time, control material nucleation and crystallization.Prepared hierarchy zinc oxide/copper oxide is received
The Large ratio surface of hierarchy, the efficient electron transfer efficiency of pore structure and ordered structure interface are combined by meter Wei Qiu, improve
The air-sensitive performance of material.Hierarchy zinc oxide/cupric oxide nano the microsphere obtained by the present invention is capable of at 125 DEG C
To H2S atmosphere sensitive, quickly detect so that the Practical Performance of this material increases.
The Preparation method and use of hierarchy zinc oxide/cupric oxide nano microsphere of the present invention, with known technology
Compare and have the advantage that and good effect:
Hierarchy zinc oxide/cupric oxide nano the microsphere prepared by the method for the invention, big by hierarchy
Specific surface, the efficient electron transfer efficiency of pore structure and ordered structure interface combine, thus improve the air-sensitive performance of material.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the present invention;
Fig. 2 is the transmission electron microscope photo of the present invention;
Fig. 3 is the X-ray diffractogram of the present invention;
Fig. 4 be the present invention under the conditions of temperature 125 DEG C to H2The calibration map of S;
Fig. 5 be the present invention under the conditions of temperature 125 DEG C to variable concentrations H2The response curve of S: 10ppb, 50ppb,
100ppb, 200ppb, 500ppb, 1000ppb, 10000ppb scheme, each concentration determination three times;
Fig. 6 be the present invention under the conditions of temperature 125 DEG C to variable concentrations H2The calibration map of S;
Fig. 7 be the present invention under the conditions of temperature 125 DEG C to variable concentrations H2The response curve of S: 200ppb, 500ppb,
1000ppb schemes.
Detailed description of the invention
The flesh and blood of the present invention is further illustrated below in conjunction with accompanying drawing.
Embodiment 1
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding by 0.0175mmol nonionic surfactant
Section copolymer is dissolved in the beaker of 9.4ml deionized water, and magnetic agitation forms uniform mixed solution in 60 minutes;
B, will in step a mixed solution add zinc nitrate hexahydrate 0.26mmol and Copper nitrate hexahydrate 0.56mmol, continue magnetic
Power stirs 30 minutes, forms uniform mixed solution;
C, step b mixed solution will add ammonium nitrate 7.7mmol, and continue magnetic agitation 40 minutes, formed uniform mixed
Close solution;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 1mm, keeps heating rate
1.0K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature after annealing 2 hours, obtains classification knot
Structure zinc oxide/cupric oxide nano microsphere, scanning electron microscope, transmission electron microscope and X-ray diffraction are shown in Fig. 1,2,3 respectively.
Embodiment 2
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding by 0.0175mmol nonionic surfactant
Section copolymer is dissolved in the beaker of 9.4ml deionized water, and magnetic agitation forms uniform mixed solution in 60 minutes;
B, step a mixed solution will add Copper nitrate hexahydrate 0.8mmol, and continue magnetic agitation 30 minutes, formed uniformly
Mixed solution;
C, mixed solution in step b will add ammonium nitrate 7.7mmol, and continue magnetic agitation 40 minutes, formed uniform
Mixed solution;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 2mm, keeps heating rate
1.0K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature after annealing 2 hours, obtains classification knot
Structure cupric oxide nano microsphere.
Embodiment 3
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding by 0.0175mmol nonionic surfactant
Section copolymer is dissolved in the beaker of 9.4ml deionized water, and magnetic agitation forms uniform mixed solution in 60 minutes;
B, will in step a mixed solution add zinc nitrate hexahydrate 0.26mmol and Copper nitrate hexahydrate 0.56mmol, continue magnetic
Power stirs 30 minutes, forms uniform mixed solution;
C, mixed solution in step b will add ammonium nitrate 7.7mmol, and continue magnetic agitation 40 minutes, formed uniform
Mixed solution;
D, the mixed solution in step c is transferred in ceramic crucible, solution height 1cm, keeps heating rate 1.0K/
Min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature, obtains hierarchy oxygen after annealing 2 hours
Change zinc/cupric oxide nano microsphere.
Embodiment 4
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding by 0.0175mmol nonionic surfactant
Section copolymer is dissolved in the beaker of 9.4ml deionized water, and magnetic agitation forms uniform mixed solution in 60 minutes,;
B, will in step a mixed solution add zinc nitrate hexahydrate 0.43mmol and Copper nitrate hexahydrate 0.45mmol, continue magnetic
Power stirs 30 minutes, forms uniform mixed solution;
C, mixed solution in step b will add ammonium chloride 7.7mmol, and continue magnetic agitation 40 minutes, formed uniform
Mixed solution;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 3mm, keeps heating rate
1.0K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature after annealing 2 hours, obtains classification knot
Structure zinc oxide/cupric oxide nano microsphere.
Embodiment 5
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) three is embedding by 0.0175mmol nonionic surfactant
Section copolymer is dissolved in the beaker of 9.4ml deionized water, and magnetic agitation forms uniform mixed solution in 60 minutes;
B, will in step a mixed solution add zinc chlorate 0.26mmol and copper chlorate 0.56mmol, continue magnetic agitation 30
Minute, form uniform mixed solution;
C, mixed solution in step b will add ammonium chlorate 7.7mmol, and continue magnetic agitation 40 minutes, formed uniform
Mixed solution;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 3mm, keeps heating rate
1.0K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature after annealing 2 hours, obtains classification knot
Structure zinc oxide/cupric oxide nano microsphere.
Embodiment 6
Detecting step:
With any one hierarchy zinc oxide and cupric oxide nano microsphere in embodiment 1-5 with cupric oxide nano microsphere it is
Example prepares sensor: take respectively the standby hierarchy zinc oxide/cupric oxide nano microsphere of 0.1 restraint and cupric oxide nano microsphere in
In agate mortar, it is separately added into 3-5 and drips deionized water, grind to form pasty state;With fine, soft fur pen, gained sample is applied to respectively 5 pectinations
On the electrode slice of electrode, form 5 sensors, electrode adds the constant current 0.45A corresponding to temperature 125 DEG C;Use Ai Li
Sensor prepared by special intelligence air-sensitive analysis system test is to H2The response curve of S.
Embodiment 7
Sensor is to H2The detection of S atmosphere:
Under the bias of 4V, the sensor obtained in testing example 6 temperature 100 DEG C, 125 DEG C, 150 DEG C to 100ppb
H2The response of S, the sensitive material wherein obtained in embodiment 1 has the performance of optimum, and corresponding response magnitude is respectively
20.6%, 30.3% and 12.1%, as shown in Figure 4.
Embodiment 8
Under the bias of 4V, the hierarchy zinc oxide/cupric oxide nano microsphere sensor obtained in testing example 1 exists
125 DEG C to variable concentrations H2S responds, and its result is as it is shown in figure 5, work as H2S adsorbs at material surface, and its resistance increases, corresponding
Response concentration be 10ppb, 50ppb, 100ppb, 200ppb, 500ppb, 1000ppb, 10000ppb its calibration result such as Fig. 6
Shown in, fit equation is R=0.048+0.0029C, and wherein R is responsiveness, is defined as the ratio of resistance change and resistance initial value,
C is H2S concentration.
Embodiment 9
Under the bias of 4V, the cupric oxide nano microsphere sensor obtained in testing example 2 temperature 125 DEG C to difference
Concentration H2S responds, and its result is as it is shown in fig. 7, work as H2S adsorbs at material surface, and its resistance increases, corresponding response concentration
For 200ppb, 500ppb, 1000ppb.
Claims (3)
1. the preparation method of hierarchy zinc oxide/cupric oxide nano microsphere, it is characterised in that follow these steps to carry out:
A, it is that poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer is dissolved in by nonionic surfactant
In deionized water, magnetic agitation forms uniform mixed solution, wherein deionized water and nonionic surfactant for 60 minutes
Mol ratio is 25000-35000:1, and in mixed solution, nonionic surfactant concentration is 0.2 mmol/L;
B, by step a mixed solution add nitrate be zinc nitrate hexahydrate and Copper nitrate hexahydrate, or chlorate be zinc chloride and
Copper chloride, continues magnetic agitation 30 minutes, forms uniform mixed solution, wherein nitrate or chlorate with step a non-from
The mol ratio of sub-surface activating agent is 20-100:1, and zinc salt is 0-1:1 with the mol ratio of mantoquita, nitrate or chlorine in mixed solution
Hydrochlorate concentration is 9.0 mmol/L;
C, it is ammonium nitrate or ammonium chloride by step b mixed solution adds ammonium salt, continues magnetic agitation 40 minutes, formed uniform
Mixed solution, wherein ammonium salt is 300-600:1 with the mol ratio of nonionic surfactant in step a, ammonium salt in mixed solution
Concentration is 0.1 mol/L;
D, being transferred in ceramic crucible by the mixed solution in step c, solution height is maintained at 1-3mm, keeps heating rate 1.0
K/min, temperature 260 DEG C is annealed 40 minutes, is continuously heating to 500 DEG C, is cooled to room temperature after annealing 2 hours, obtains classification knot
Structure zinc oxide/cupric oxide nano microsphere.
The preparation method of hierarchy zinc oxide/cupric oxide nano microsphere the most according to claim 1, it is characterised in that step
The mass ratio obtaining the zinc oxide in hierarchy zinc oxide/cupric oxide nano microsphere and copper oxide in rapid d is 1:2.
Hierarchy zinc oxide/cupric oxide nano microsphere that method the most according to claim 1 obtains quickly is detecting ppb
Concentration H2Purposes in S atmosphere.
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Cited By (2)
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CN107537501A (en) * | 2017-08-28 | 2018-01-05 | 武汉理工大学 | A kind of hierarchical Z nO/CuO composites and preparation method thereof |
CN114506873A (en) * | 2022-01-14 | 2022-05-17 | 河北工业大学 | CuO/ZnO nano material derived from metal organic framework and preparation method and application thereof |
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CN104955771A (en) * | 2013-01-31 | 2015-09-30 | 国立大学法人大阪大学 | Metal oxide mesocrystal, and method for producing same |
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CN102259907A (en) * | 2011-06-30 | 2011-11-30 | 上海大学 | Porous zinc oxide nano material and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107537501A (en) * | 2017-08-28 | 2018-01-05 | 武汉理工大学 | A kind of hierarchical Z nO/CuO composites and preparation method thereof |
CN107537501B (en) * | 2017-08-28 | 2020-08-04 | 武汉理工大学 | ZnO/CuO composite material with hierarchical structure and preparation method thereof |
CN114506873A (en) * | 2022-01-14 | 2022-05-17 | 河北工业大学 | CuO/ZnO nano material derived from metal organic framework and preparation method and application thereof |
CN114506873B (en) * | 2022-01-14 | 2024-01-16 | 河北工业大学 | Metal organic framework derived CuO/ZnO nano material and preparation method and application thereof |
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Application publication date: 20161109 |