CN107555400B - Gas sensor ferric oxide nano ring/nickel oxide composite material - Google Patents
Gas sensor ferric oxide nano ring/nickel oxide composite material Download PDFInfo
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- CN107555400B CN107555400B CN201710618353.1A CN201710618353A CN107555400B CN 107555400 B CN107555400 B CN 107555400B CN 201710618353 A CN201710618353 A CN 201710618353A CN 107555400 B CN107555400 B CN 107555400B
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Abstract
The present invention provides a kind of gas sensor ferric oxide nano ring/nickel oxide composite material, deionized water is dissolved in by soluble ferric iron salt, soluble nickel salt, add trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution, magnetic agitation, it is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, ferric oxide nano ring/nickel oxide composite material pre-burning powder is obtained, calcining obtains ferric oxide nano ring/nickel oxide composite material.The present invention uses one step hydro thermal method to prepare using ferric oxide nano ring as carrier, ferric oxide nano ring/nickel oxide composite material of flower-shaped nickel oxide is grown in ferric oxide nano ring surfaces externally and internally, preparation method is simple, controllable adjustment ferric oxide nano ring size dimension, ferric oxide nano ring/nickel oxide composite material large specific surface area, the advantage for greatly having played nickel oxide, can be used for the preparation of gas sensor.This method reaction time is short simultaneously, and yield is high, can prepare in batches to be suitble to industrial-scale production.
Description
Technical field
The present invention relates to gas sensor field of material preparation, specially a kind of gas sensor with ferric oxide nano ring/
Nickel oxide composite material, the invention further relates to its applications.
Technical background
Since the 21th century, people's environmental pollution and energy shortage problem are increasingly paid close attention to, for this two side
The scientific research in face is also more and more, and nickel oxide is a kind of common metal oxide, due to its excellent performance, nickel oxide quilt
It is widely used in the fields such as photochemical catalyst, gas sensitive material, dielectric material.Wherein, nickel oxide is weight in gas sensitive material
The one kind wanted improves its specific surface area in conjunction with stronger exchange of particles performance, is conducive to reactant in catalytic process in activity
Position is reacted, to H2S, greatly application prospect is shown in terms of the detection of the gases such as ethyl alcohol, acetone, formaldehyde.However, single
The air-sensitive performance of nickel oxide material is controlled by pattern, crystal form, specific surface area of material etc., low, poor selectivity that there are still sensitivity
The disadvantages of.Fe2O3It is a kind of common material, there are many patterns, by Fe2O3Nano-rings promote nickel oxide to exist in conjunction with nickel oxide
Fe2O3The surfaces externally and internally of nano-rings is formed, and specific surface area can be effectively improved, and promotes the air-sensitive performance of composite material.
The present invention uses one step hydro thermal method, and simple process is easy to control, and can be formed not in Fe2O3 nano-rings surfaces externally and internally
With the nickel oxide of pattern, the air-sensitive performance of specific surface area and material is greatly promoted.At the same time, scale can be achieved in yield height
Production.
Summary of the invention
To overcome the above the deficiencies in the prior art, the present invention is to solve: a kind of gas sensor iron oxide is provided
Nano-rings/nickel oxide composite material, by the unique Fe of pattern2O3Nanometer ring material and nickel oxide form composite material.
Another object of the present invention is: providing the application of above-mentioned ferric oxide nano ring/nickel oxide composite material.
The object of the invention is realized by following proposal: a kind of gas sensor ferric oxide nano ring/nickel oxide composite wood
Material, comprising the following steps:
(1) weigh soluble ferric iron salt respectively, soluble nickel salt is dissolved in deionized water, be made into mixed solution, wherein mixing it is molten
Liquid Fe3+The concentration of salt is 0.005 ~ 0.025 mol/L, Ni2+The concentration of salt is 0.005 ~ 0.1 mol/L；
(2) trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution are added, wherein lemon
Sour trisodium and the molar ratio of nickel salt are 1.1 ~ 1.5:1, and hexa and nickel salt molar ratio are 1 ~ 2:1, and sodium sulphate is mixing
Concentration in solution is 1.0 × 10-5~4.0×10-4 Mol/L, ammonium dihydrogen phosphate add the concentration in mixed solution be 1.0 ×
10-4~5.0×10-4 Mol/L, the uniform mixed liquor of magnetic agitation；
(3) hydro-thermal reaction, the uniform mixed liquor of magnetic agitation are transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, water
Thermal response temperature is 140 ~ 240 DEG C, and the reaction time is to obtain ferric oxide nano ring/nickel oxide composite material pre-burning powder in 4 ~ 24 hours
Body；
(4) it calcines, obtains ferric oxide nano ring/nickel oxide composite material.
The characteristics of ferric oxide nano ring/nickel oxide composite material of the present invention is: nickel oxide is in Fe2O3Nano-rings surfaces externally and internally
It is formed, the air-sensitive performance of specific surface area and composite material can be effectively improved.
On the basis of above scheme, the soluble ferric iron salt is iron chloride or ferric nitrate, and the soluble nickel salt is
Nickel nitrate, nickel chloride or nickel acetate.
On the basis of above scheme, magnetic agitation speed is 100 ~ 1000 rpm, and mixing time is 1 ~ 12 hour.
On the basis of above scheme, calcination temperature is 300 ~ 400 DEG C, and calcination time is 1 ~ 6 hour.
The present invention provides a kind of to be answered according to above-mentioned gas sensor ferric oxide nano ring/nickel oxide composite material
With.
Compared with prior art, the present invention there is following benefit:
1. one step hydro thermal method prepares Fe2O3Nano-rings are ferric oxide nano ring/nickel oxide composite material of carrier, wherein
Nickel oxide is in Fe2O3Nano-rings surfaces externally and internally is formed, and the specific surface area of composite material can be effectively improved, to promote its gas sensing property
Energy.
2. the composite material pattern is unique, do not reported in other documents.
3. simple process, the morphology controllable of composite material, yield is high, it is produced on a large scale.
Detailed description of the invention:
Fig. 1 is Fe2O3The shape appearance figure of nano-rings SEM × 100000；
Fig. 2 is ferric oxide nano ring/nickel oxide composite material TEM shape appearance figure.
Specific embodiment
A specific embodiment of the invention is explained in detail below with reference to embodiment, but the present invention can be with very much
Implement different from other modes described herein, therefore the present invention is not limited to the specific embodiments disclosed below.It please refers to
Fig. 1 is Fe2O3The shape appearance figure of nano-rings SEM × 100000 and Fig. 2 are ferric oxide nano ring/nickel oxide composite material TEM shape appearance figure.
Embodiment 1
The preparation of ferric oxide nano ring/nickel oxide composite material:
(1) iron chloride is weighed, nickel nitrate is dissolved in deionized water, is made into mixed solution, wherein mixed solution Fe3+The concentration of salt
For 0.005 mol/L, Ni2+The concentration of salt is 0.005 mol/L；
(2) trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution are added, wherein citric acid
Trisodium and the molar ratio of nickel salt are 1.1:1, and hexa and nickel salt molar ratio are 2:1, and sodium sulphate is in mixed solution
Concentration is 4.0 × 10-4 Mol/L, it is 1.0 × 10 that ammonium dihydrogen phosphate, which adds the concentration in mixed solution,-4 Mol/L, magnetic agitation
Rate is 800 rpm, and mixing time is 10 hours；
(3) hydro-thermal reaction: the above mixed solution is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, controls hydro-thermal
Reaction temperature is 150 DEG C, and the reaction time is 24 hours, obtains ferric oxide nano ring/nickel oxide composite material pre-burning powder；
(4) it calcines: being calcined 6 hours at 300 DEG C, obtain ferric oxide nano ring/nickel oxide composite material.
Please referring to Fig. 1 is Fe2O3The shape appearance figure of nano-rings SEM × 100000 and Fig. 2 are that ferric oxide nano ring/nickel oxide is compound
Material TEM shape appearance figure, nickel oxide is in Fe2O3Nano-rings surfaces externally and internally is formed.
Embodiment 2
The preparation of ferric oxide nano ring/nickel oxide composite material:
(1) ferric nitrate etc. is weighed, nickel chloride etc. is dissolved in deionized water, is made into mixed solution, wherein mixed solution Fe3+Salt
Concentration is 0.02 mol/L, Ni2+The concentration of salt is 0.05 mol/L；
(2) trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution are added, wherein citric acid
Trisodium and the molar ratio of nickel salt are 1.2:1, and hexa and nickel salt molar ratio are 1:1, and sodium sulphate is in mixed solution
Concentration is 1.0 × 10-5Mol/L, it is 5.0 × 10 that ammonium dihydrogen phosphate, which adds the concentration in mixed solution,-4 Mol/L, magnetic agitation
Rate is 100 rpm, and mixing time is 12 hours；
(3) hydro-thermal reaction: the above mixed solution is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, controls hydro-thermal
Reaction temperature is 140 DEG C, and the reaction time is 12 hours, obtains ferric oxide nano ring/nickel oxide composite material pre-burning powder；
(4) it calcines: being calcined 4 hours at 350 DEG C, obtain ferric oxide nano ring/nickel oxide composite material.
Embodiment 3
The preparation of ferric oxide nano ring/nickel oxide composite material:
(1) iron chloride is weighed, nickel acetate etc. is dissolved in deionized water, is made into mixed solution, wherein mixed solution Fe3+Salt it is dense
Degree is 0.005 mol/L, Ni2+The concentration of salt is 0.1 mol/L；
(2) trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution are added, wherein citric acid
Trisodium and the molar ratio of nickel salt are 1.5:1, and hexa and nickel salt molar ratio are 1.5:1, and sodium sulphate is in mixed solution
Concentration be 3.0 × 10-4 Mol/L, it is 3 × 10 that ammonium dihydrogen phosphate, which adds the concentration in mixed solution,-4 Mol/L, magnetic agitation
Rate is 1000 rpm, and mixing time is 1 hour；
(3) hydro-thermal reaction: the above mixed solution is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, controls hydro-thermal
Reaction temperature is 240 DEG C, and the reaction time is 4 hours, obtains ferric oxide nano ring/nickel oxide composite material pre-burning powder；
(4) it calcines: being calcined 1 hour at 400 DEG C, obtain ferric oxide nano ring/nickel oxide composite material.
Claims (5)
1. a kind of gas sensor ferric oxide nano ring/nickel oxide composite material, comprising the following steps:
(1) weigh soluble ferric iron salt respectively, soluble nickel salt is dissolved in deionized water, be made into mixed solution, wherein mixed solution Fe3 +The concentration of salt is 0.005 ~ 0.025 mol/L, Ni2+The concentration of salt is 0.005 ~ 0.1 mol/L；
(2) trisodium citrate, hexa, sodium sulphate, ammonium dihydrogen phosphate to mixed solution are added, wherein citric acid three
The molar ratio of sodium and nickel salt is 1.1 ~ 1.5:1, and hexa and nickel salt molar ratio are 1 ~ 2:1, and sodium sulphate is in mixed solution
In concentration be 1.0 × 10-5~4.0×10-4 Mol/L, it is 1.0 × 10 that ammonium dihydrogen phosphate, which adds the concentration in mixed solution,-4~
5.0×10-4 Mol/L obtains uniform mixed liquor using magnetic agitation；
(3) hydro-thermal reaction, the uniform mixed liquor of magnetic agitation are transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, and hydro-thermal is anti-
Answering temperature is 140 ~ 240 DEG C, and the reaction time is to obtain ferric oxide nano ring/nickel oxide composite material pre-burning powder in 4 ~ 24 hours；
(4) it calcines, obtains ferric oxide nano ring/nickel oxide composite material.
2. gas sensor ferric oxide nano ring/nickel oxide composite material according to claim 1, which is characterized in that institute
The soluble ferric iron salt stated is iron chloride or ferric nitrate, and the soluble nickel salt is nickel nitrate, nickel chloride or nickel acetate.
3. gas sensor ferric oxide nano ring/nickel oxide composite material according to claim 1, which is characterized in that magnetic
Power stirring rate is 100 ~ 1000 rpm, and mixing time is 1 ~ 12 hour.
4. gas sensor ferric oxide nano ring/nickel oxide composite material according to claim 1, which is characterized in that forge
Burning temperature is 300 ~ 400 DEG C, and calcination time is 1 ~ 6 hour.
5. one kind is answered to gas sensor ferric oxide nano ring/nickel oxide composite material described in 4 according to claim 1
With.
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