CN107867714A - Nanocrystalline SnO2/ graphene composite air-sensitive material and preparation method thereof - Google Patents

Nanocrystalline SnO2/ graphene composite air-sensitive material and preparation method thereof Download PDF

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Publication number
CN107867714A
CN107867714A CN201711015059.8A CN201711015059A CN107867714A CN 107867714 A CN107867714 A CN 107867714A CN 201711015059 A CN201711015059 A CN 201711015059A CN 107867714 A CN107867714 A CN 107867714A
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nanocrystalline
graphene
sensitive material
sno
preparation
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官群
王斌
程建丽
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Institute of Chemical Material of CAEP
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • 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
    • 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

Abstract

The invention discloses a kind of Nanocrystalline SnO2/ graphenes composite air-sensitive material, and load skeleton, Nanocrystalline SnO are used as using single-layer graphene2Original position is embedded in the both sides and edge of graphene, SnO2Nanocrystalline is 5~20nm, Nanocrystalline SnO2/ graphene complex material is stacked in sandwich shape.The invention also discloses the Nanocrystalline SnO of a kind of high efficiency, low cost2The preparation method of/graphene composite air-sensitive material.The Nanocrystalline SnO of the present invention2/ graphene composite air-sensitive material, can improve SnO2Electric conductivity, reduce response temperature, improve the performance such as response stability.

Description

Nanocrystalline SnO2/ graphene composite air-sensitive material and preparation method thereof
Technical field
The present invention relates to a kind of to highly sensitive response gas sensitive of nitrogen oxides and preparation method thereof, and in particular to a kind of Nanocrystalline SnO2/ graphene composite air-sensitive material and preparation method thereof.
Background technology
In daily life, poisonous gas caused by burning, blast, leakage etc., such as：NOx、SOx、CoO、H2Etc. spreading in sky In gas, the healthy living of people is had a strong impact on.Especially NO2, its concentration may result in poisoning when being more than 20ppm.For harmful The detection means and method of gas, bring into schedule already, and society also increasingly increases the demand for monitoring this respect, many scientists Put forth effort to research and develop the selective high, gas sensor of high sensitivity.
In recent years, researcher furthers investigate in gas sensor Material Field, particularly to semiconductor gas sensitive quite For concern, such as SnO2、ZnO、WO3、GuO、Fe2O3Deng by the way that physical absorption and chemical reaction occurs with detected gas, causing Carrier moving inside semi-conducting material, causes the generations such as resistance, electric current to change accordingly, so as to reach detection toxic noxious gas The presence of body.
Semiconductor gas sensors material is divided into two kinds of p-type and N-type.N-type semiconductor detection oxidizing gas resistance becomes big, and detection is also Originality gas resistance diminishes；P-type semiconductor is just opposite with N-type semiconductor.SnO2A kind of N-type broad stopband as stabilization (3.67eV) semi-conducting material, is widely used in gas sensor, has high sensitivity, fast response time, stability etc. very More excellent properties.But many urgent problems to be solved are also run into actual applications, as resistance is big, operating temperature is high, selection Property difference etc..
The content of the invention
An object of the present invention is to provide a kind of high sensitivity, fast response time, operating temperature low composite gas Responsive materials.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of Nanocrystalline SnO2/ graphenes composite air-sensitive material, load skeleton, Nanocrystalline are used as using single-layer graphene SnO2Original position is embedded in the both sides and edge of graphene, SnO2Nanocrystalline is 5~20nm, Nanocrystalline SnO2/ graphene complex Nanocrystalline SnO in material2, single-layer graphene, Nanocrystalline SnO2It is stacked in sandwich shape.
It is another object of the present invention to provide the Nanocrystalline SnO of a kind of high efficiency, low cost2/ graphene is compound The preparation method of gas sensitive.
A kind of Nanocrystalline SnO2The preparation method of/graphene composite air-sensitive material
Nanocrystalline SnO2The preparation method of/graphene composite air-sensitive material, is concretely comprised the following steps：
A, graphite oxide is prepared using modified Hummers methods；
B, by the graphite oxide ultrasonic disperse obtained by step a to deionized water, graphene oxide water solution is obtained；
C, absolute ethyl alcohol and polyethylene glycol are stirred according to certain volume ratio, obtain mixed solvent；
D, anhydrous oxalic acid is dissolved in the in the mixed solvent in step c, stirs, obtain oxalic acid solution；
E, stannous chloride is hydrated by two, be dissolved in the oxalic acid solution in step d, stirred to being completely dissolved, obtain transparent Tin-salt solution；
F, the graphene oxide water solution in step b is added dropwise in the tin-salt solution in step e, stirs 1-10h, it is quiet Only, precipitation is collected；
G, the precipitation drying for obtaining step f, grinding, obtains the presoma of compound；
H, the powdered compound precursor for obtaining step f process annealing in high-vacuum environment.
Graphite oxide is prepared with reference to Hummers methods in above-mentioned steps a.It is to pre-oxidize first, a certain amount of concentrated sulfuric acid, mistake Potassium sulfate, phosphorus pentoxide are well mixed, and heating, are then added 5g graphite powders, are obtained dark blue mixture, filtering and washing to pH =5~12,80 DEG C are dried in vacuum overnight.Secondly, 2.5g pre-oxidation graphite is weighed, the concentrated sulfuric acid is added under ice bath, then by 7.5g Potassium permanganate is slowly added into mixed solution and 20 DEG C of 2.5h stirred below of keeping temperature, adds deionized water and stirs 1.5h, add 30%H2O2Terminate to reaction.Obtained product is respectively washed 3 times with watery hydrochloric acid and deionized water, obtains graphite oxide water Solution, freeze-drying obtain graphite oxide.
Water bath sonicator is to peel off graphite oxide, obtaining single-layer graphene oxide in above-mentioned steps b.
The volume ratio of the mixed solvent obtained in above-mentioned steps c, absolute ethyl alcohol and polyethylene glycol should be 5:1~1:5.
Anhydrous oxalic acid is dissolved in step c in the mixed solvents by above-mentioned steps d, and concentration of oxalic acid is 0.08~0.02g/mL.
Two hydration stannous chloride are dissolved in step d oxalic acid mixed solutions by above-mentioned steps e, and its concentration is 8~30mg/mL.
Magnetic agitation mixing is mixed into above-mentioned steps f or is ultrasonically treated one kind of mixing.
Graphene oxide is added dropwise in step e solution in above-mentioned steps f, graphene oxide and SnCl2·2H2O quality Than for 2:1~5:1.
Dried in above-mentioned steps g as freeze-drying or vacuum drying one kind.
Be annealed into above-mentioned steps h vacuum less than 50Pa vacuum environment under, less than 450 DEG C in a low temperature of preserve 30min~120min.
Same SnO2Single phase ratio, nano composite material prepared by this method have the characteristics that：
(1) preparation technology cheap and simple, the preparation of Nanocrystalline SnO2/ graphene composite air-sensitive materials is to pass through wet-chemical Precipitation and cryogenic vacuum are annealed and obtained, and cost is low, and synthesis technique is simple, short preparation period, efficiency high, green non-poisonous, avoids Environmental pollution.
(2) the Nanocrystalline SnO prepared2The design feature of the compound sensitive material of/graphene is Nanocrystalline SnO2Uniformly Ground is embedded on graphene, it is suppressed that SnO2Reunite and lump, add the specific surface area of sensitive material, be advantageous to adsorb titanium dioxide Nitrogen.Simultaneously as graphene has excellent electric conductivity, good thermal conductivity and ductility, composite wood is significantly improved The structural stability of material, reduce response temperature, selection performance of the raising to atmosphere.
The Nanocrystalline SnO of the present invention2/ graphene composite air-sensitive material, it is typically characterized by 5~20nm Nanocrystallines SnO2Graphene both sides and edge and hole are embedded in, form a kind of Two-dimensional Composites.And as the substrate in composite, Graphene has the characteristics of excellent electric conductivity and high-specific surface area, Nanocrystalline SnO again2Graphite can be supported on by original position On alkene lamella, SnO is improved with this2Electric conductivity, reduce response temperature, improve the performance such as response stability.
Brief description of the drawings
Fig. 1 is Nanocrystalline SnO2The TEM figures of/graphene composite air-sensitive material.
Fig. 2 is the Nanocrystalline SnO of different content at 30 DEG C2Graphene composite material is loaded to various concentrations NO2Response Scheme (MGO:MSn=1:1；MGO:MSn=2:1；MGO:MSn=5:1).
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with the accompanying drawings and embodiment, it is right The present invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not For limiting the present invention.
Embodiment one
With GO and SnCl2·2H2O mass ratio is 2:1 prepares nanocrystal shape SnO2/ graphene complex response material
By absolute ethyl alcohol and polyethylene glycol with volume ratio 3:2 are uniformly mixed, and take 1mL mixed solutions, then by two water Close stannous chloride (SnCl2·2H2O) 0.02g is dissolved in mixed solution, after stirring 1h, is slowly added dropwise to graphene oxide 8mL (graphene oxide concentration is：5mg/mL), 1h is stirred by ultrasonic, it is static, precipitation is collected by centrifugation, absolute ethyl alcohol and deionized water are respectively washed Wash 3 times, freeze-drying obtains composite precursor.Finally, under 20Pa vacuums, 400 DEG C of insulation 1h, compound produce are obtained Product.
The product addition absolute ethyl alcohol ground and mixed of collection is uniform, slurry is applied in interdigital electrode, 80 DEG C of agings 2-5 days, it is subsequently placed in the test of air-sensitive tester.By test it is known that under 1ppm nitrogen dioxide atmosphere, Nanocrystalline SnO2The sensitivity at 30 DEG C of/graphene complex response material is 26, recovery time 504s.
Embodiment two
With GO and SnCl2·2H2O mass ratio is 1:1 prepares nanocrystal shape SnO2/ graphene complex response material
By absolute ethyl alcohol and polyethylene glycol with volume ratio 2:1 is uniformly mixed, and takes 1mL mixed solutions, then by two water Close stannous chloride (SnCl2·2H2O) 0.02g is dissolved in mixed solution, after stirring 1h, is slowly added dropwise to graphene oxide 4mL (graphene oxide concentration is：5mg/mL), 1h is stirred by ultrasonic, it is static, precipitation is collected by centrifugation, absolute ethyl alcohol and deionized water are respectively washed Wash 3 times, vacuum drying obtains compound precursor.Finally, under 20Pa vacuums, 300 DEG C of insulation 1h, compound produce are obtained Product.
The product addition absolute ethyl alcohol ground and mixed of collection is uniform, slurry is applied in interdigital electrode, 80 DEG C of agings 2-5 days, it is subsequently placed in the test of air-sensitive tester.By test it is known that under 1ppm nitrogen dioxide atmosphere, Nanocrystalline SnO2The sensitivity at 30 DEG C of/graphene complex response material is 23, recovery time 627.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferable embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art Member can be designed that a lot of other modifications and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application Within scope and spirit.

Claims (10)

  1. A kind of 1. Nanocrystalline SnO2/ graphene composite air-sensitive material, it is characterised in that：Using single-layer graphene as load skeleton, Nanocrystalline SnO2Original position is embedded in the both sides and edge of graphene, SnO2Nanocrystalline is 5~20nm, Nanocrystalline SnO2/ graphite Nanocrystalline SnO in alkene composite materials2, single-layer graphene, Nanocrystalline SnO2It is stacked in sandwich shape.
  2. A kind of 2. Nanocrystalline SnO2The preparation method of/graphene composite air-sensitive material, it is characterised in that：Concretely comprise the following steps：
    A, graphite oxide is prepared using modified Hummers methods；
    B, by the graphite oxide ultrasonic disperse obtained by step a to deionized water, graphene oxide water solution is obtained；
    C, absolute ethyl alcohol and polyethylene glycol are stirred according to certain volume ratio, obtain mixed solvent；
    D, anhydrous oxalic acid is dissolved in the in the mixed solvent in step c, stirs, obtain oxalic acid solution；
    E, stannous chloride is hydrated by two, be dissolved in the oxalic acid solution in step d, stirred to being completely dissolved, obtain transparent pink salt Solution；
    F, the graphene oxide water solution in step b is added dropwise in the tin-salt solution in step e, stirs 1-10h, it is static, receive Collection precipitation；
    G, the precipitation drying for obtaining step f, grinding, obtains the presoma of compound；
    H, the powdered compound precursor for obtaining step f process annealing in high-vacuum environment.
  3. 3. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Graphite oxide is prepared with reference to Hummers methods in step a.First be pre-oxidation, a certain amount of concentrated sulfuric acid, potassium peroxydisulfate, Phosphorus pentoxide is well mixed, and heating, is then added 5g graphite powders, is obtained dark blue mixture, and filtering and washing to pH=5~ 12,80 DEG C are dried in vacuum overnight.Secondly, 2.5g pre-oxidation graphite is weighed, the concentrated sulfuric acid is added under ice bath, then by 7.5g permanganic acid Potassium is slowly added into mixed solution and 20 DEG C of 2.5h stirred below of keeping temperature, adds deionized water and stirs 1.5h, adds 30%H2O2Terminate to reaction.Obtained product is respectively washed 3 times with watery hydrochloric acid and deionized water, obtains the graphite oxide aqueous solution, freezing It is dried to obtain graphite oxide.
  4. 4. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    The volume ratio of the mixed solvent obtained in step c, absolute ethyl alcohol and polyethylene glycol is 5:1~1:5.
  5. 5. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Anhydrous oxalic acid is dissolved in step c in the mixed solvents by step d, and concentration of oxalic acid is 0.08~0.02g/mL.
  6. 6. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Two hydration stannous chloride are dissolved in step d oxalic acid mixed solutions by step e, and its concentration is 8~30mg/mL.
  7. 7. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Magnetic agitation mixing is mixed into step f or is ultrasonically treated one kind of mixing.
  8. 8. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Graphene oxide is added dropwise in step e solution in step f, graphene oxide and SnCl2·2H2O mass ratio is 2:1 ~5:1.
  9. 9. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Dried in step g as freeze-drying or vacuum drying one kind.
  10. 10. Nanocrystalline SnO according to claim 22The preparation method of/graphene composite air-sensitive material, it is characterised in that：
    Be annealed into step h vacuum less than 50Pa vacuum environment under, less than 450 DEG C in a low temperature of preserve 30min~ 120min。
CN201711015059.8A 2017-10-26 2017-10-26 Nanocrystalline SnO2/ graphene composite air-sensitive material and preparation method thereof Pending CN107867714A (en)

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CN108598428A (en) * 2018-04-26 2018-09-28 东华大学 A kind of graphene/stannic oxide alternating layers stack composite fibre and its preparation method and application
CN108807962A (en) * 2018-07-31 2018-11-13 澳洋集团有限公司 A kind of preparation method of stannic oxide-graphene negative material
CN108956712A (en) * 2018-06-29 2018-12-07 五邑大学 ZnO nano crystalline substance enhances Si nano column array sensitive material and preparation method thereof and sensor
CN110498405A (en) * 2019-08-21 2019-11-26 南京倍格电子科技有限公司 A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof
CN113336263A (en) * 2021-06-23 2021-09-03 陕西科技大学 Mesoporous SnO2Nanorod/nitrogen-doped graphene composite sensitive material and preparation method and application thereof
CN114094062A (en) * 2021-10-09 2022-02-25 温州大学 Preparation method and application of oxalic acid assisted synthesis of tin dioxide nanoparticle composite graphene high-performance lithium storage and sodium storage material
CN115466973A (en) * 2022-09-09 2022-12-13 天津科技大学 Calcium stannate-tin oxide/conductive carbon black nano catalyst and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108598428A (en) * 2018-04-26 2018-09-28 东华大学 A kind of graphene/stannic oxide alternating layers stack composite fibre and its preparation method and application
CN108956712A (en) * 2018-06-29 2018-12-07 五邑大学 ZnO nano crystalline substance enhances Si nano column array sensitive material and preparation method thereof and sensor
CN108956712B (en) * 2018-06-29 2021-01-12 五邑大学 ZnO nanocrystal enhanced Si nanorod array sensitive material, preparation method thereof and sensor
CN108807962A (en) * 2018-07-31 2018-11-13 澳洋集团有限公司 A kind of preparation method of stannic oxide-graphene negative material
CN110498405A (en) * 2019-08-21 2019-11-26 南京倍格电子科技有限公司 A kind of graphene/tin oxide composite air-sensitive material and preparation method thereof
CN113336263A (en) * 2021-06-23 2021-09-03 陕西科技大学 Mesoporous SnO2Nanorod/nitrogen-doped graphene composite sensitive material and preparation method and application thereof
CN114094062A (en) * 2021-10-09 2022-02-25 温州大学 Preparation method and application of oxalic acid assisted synthesis of tin dioxide nanoparticle composite graphene high-performance lithium storage and sodium storage material
CN114094062B (en) * 2021-10-09 2024-04-05 温州大学 Preparation method and application of high-performance lithium and sodium storage material for synthesizing tin dioxide nanoparticle composite graphene with assistance of oxalic acid
CN115466973A (en) * 2022-09-09 2022-12-13 天津科技大学 Calcium stannate-tin oxide/conductive carbon black nano catalyst and preparation method thereof

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