CN107555400A - 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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- CN107555400A CN107555400A CN201710618353.1A CN201710618353A CN107555400A CN 107555400 A CN107555400 A CN 107555400A CN 201710618353 A CN201710618353 A CN 201710618353A CN 107555400 A CN107555400 A CN 107555400A
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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, the size dimension of controllable adjustment ferric oxide nano ring, ferric oxide nano ring/nickel oxide composite material specific surface area is big, the advantage of nickel oxide, the preparation available for gas sensor are greatly played.This method reaction time is short simultaneously, and yield is high, can prepare in batches to be adapted 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 application.
Technical background
Since 21 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, improve its specific surface area and combine stronger exchange of particles performance, be advantageous to reactant in catalytic process in activity
Position is reacted, to H2S, greatly application prospect is shown in terms of the detection of the gas such as ethanol, acetone, formaldehyde.It is however, single
The air-sensitive performance of nickel oxide material is controlled by pattern, crystal formation, specific surface area of material etc., still suffers from that sensitivity is low, poor selectivity
The shortcomings of.Fe2O3It is a kind of common material, there are different morphologies, by Fe2O3Nano-rings are combined with nickel oxide, promote nickel oxide to exist
Fe2O3The surfaces externally and internally of nano-rings is formed, and can effectively improve specific surface area, lifts the air-sensitive performance of composite.
The present invention uses one step hydro thermal method, and technique is simple, is easily controlled, and can be formed not in Fe2O3 nano-rings surfaces externally and internally
With the nickel oxide of pattern, the greatly air-sensitive performance of lifting specific surface area and material.At the same time, the high achievable scale of yield
Production.
The content of the invention
To overcome 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 forms composite with nickel oxide.
Another object of the present invention is：The application of above-mentioned ferric oxide nano ring/nickel oxide composite material is provided.
The object of the invention is realized by following proposal：A kind of gas sensor ferric oxide nano ring/nickel oxide composite wood
Material, comprises 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 are added to mixed solution, wherein, citric acid three
The mol ratio of sodium and nickel salt is 1.1 ~ 1.5:1, hexa is 1 ~ 2 with nickel salt mol ratio:1, sodium sulphate is in mixed solution
In concentration be 1.0 × 10-5~4.0×10-4 Mol/L, the concentration that ammonium dihydrogen phosphate adds in mixed solution are 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, and hydro-thermal is anti-
It is 140 ~ 240 DEG C to answer temperature, and the reaction time is to obtain ferric oxide nano ring/nickel oxide composite material pre-burning powder in 4 ~ 24 hours；
（4）Calcining, 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
Formed, the air-sensitive performance of specific surface area and composite can be effectively improved.
On the basis of such scheme, described soluble ferric iron salt is iron chloride or ferric nitrate, and described soluble nickel salt is
Nickel nitrate, nickel chloride or nickel acetate.
On the basis of such scheme, magnetic agitation speed is 100 ~ 1000 rpm, and mixing time is 1 ~ 12 hour.
On the basis of such scheme, calcining heat is 300 ~ 400 DEG C, and calcination time is 1 ~ 6 hour.
The present invention provides a kind of answering with ferric oxide nano ring/nickel oxide composite material according to above-mentioned gas sensor
With.
The present invention compared with prior art, there is following benefit：
1. one step hydro thermal method prepares Fe2O3Nano-rings are ferric oxide nano ring/nickel oxide composite material, wherein oxygen of carrier
Change nickel in Fe2O3Nano-rings surfaces externally and internally is formed, and can effectively improve the specific surface area of composite, so as to lift its air-sensitive performance.
2. the composite pattern is unique, do not reported in other documents.
3. technique is simple, the morphology controllable of composite, yield is high, is produced on a large scale.
Brief description of the drawings：
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 figures.
Embodiment
The embodiment of the present invention is explained with reference to embodiment, but the present invention can be with a lot
Implement different from other modes described here, therefore the present invention is not limited to the specific embodiments disclosed below.Refer 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 figures.
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 is
0.005 mol/L, Ni2+The concentration of salt is 0.005 mol/L；
（2）Add trisodium citrate, hexa, sodium sulphate, wherein ammonium dihydrogen phosphate to mixed solution, trisodium citrate
Mol ratio with nickel salt is 1.1:1, hexa is 2 with nickel salt mol ratio:1, concentration of the sodium sulphate in mixed solution
For 4.0 × 10-4 Mol/L, the concentration that ammonium dihydrogen phosphate adds in mixed solution are 1.0 × 10-4 Mol/L, magnetic agitation speed
For 800 rpm, mixing time is 10 hours；
（3）Hydro-thermal reaction：Solution mixed above 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）Calcining：Calcined 6 hours at 300 DEG C, obtain ferric oxide nano ring/nickel oxide composite material.
It is Fe to refer to Fig. 12O3The 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 figures, 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 it is dense
Spend for 0.02 mol/L, Ni2+The concentration of salt is 0.05 mol/L；
（2）Add trisodium citrate, hexa, sodium sulphate, wherein ammonium dihydrogen phosphate to mixed solution, trisodium citrate
Mol ratio with nickel salt is 1.2:1, hexa is 1 with nickel salt mol ratio:1, concentration of the sodium sulphate in mixed solution
For 1.0 × 10-5Mol/L, the concentration that ammonium dihydrogen phosphate adds in mixed solution are 5.0 × 10-4 Mol/L, magnetic agitation speed
For 100 rpm, mixing time is 12 hours；
（3）Hydro-thermal reaction：Solution mixed above 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）Calcining：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+The concentration of salt
For 0.005 mol/L, Ni2+The concentration of salt is 0.1 mol/L；
（2）Add trisodium citrate, hexa, sodium sulphate, wherein ammonium dihydrogen phosphate to mixed solution, trisodium citrate
Mol ratio with nickel salt is 1.5:1, hexa is 1.5 with nickel salt mol ratio:1, sodium sulphate is dense in mixed solution
Spend for 3.0 × 10-4 Mol/L, the concentration that ammonium dihydrogen phosphate adds in mixed solution are 3 × 10-4 Mol/L, magnetic agitation speed
For 1000 rpm, mixing time is 1 hour；
（3）Hydro-thermal reaction：Solution mixed above 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）Calcining：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, comprises 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 are added to mixed solution, wherein, citric acid three
The mol ratio of sodium and nickel salt is 1.1 ~ 1.5:1, hexa is 1 ~ 2 with nickel salt mol ratio:1, sodium sulphate is in mixed solution
In concentration be 1.0 × 10-5~4.0×10-4 Mol/L, the concentration that ammonium dihydrogen phosphate adds in mixed solution are 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, and hydro-thermal is anti-
It is 140 ~ 240 DEG C to answer temperature, and the reaction time is to obtain ferric oxide nano ring/nickel oxide composite material pre-burning powder in 4 ~ 24 hours；
（4）Calcining, obtains ferric oxide nano ring/nickel oxide composite material.
2. gas sensor ferric oxide nano ring/nickel oxide composite material according to claim 1, it is characterised in that institute
The soluble ferric iron salt stated is iron chloride or ferric nitrate, and described 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, it is characterised in that magnetic
Power stir speed (S.S.) 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, it is characterised in that forge
It is 300 ~ 400 DEG C to burn temperature, and calcination time is 1 ~ 6 hour.
5. a kind of gas sensor according to Claims 1-4 should with ferric oxide nano ring/nickel oxide composite material
With.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112551635A (en) * | 2020-12-11 | 2021-03-26 | 宁波市疾病预防控制中心 | Boron nitride quantum dot modified nano annular magnetic graphene oxide composite photocatalytic material and preparation method and application thereof |
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