CN109110803A - More chemical state PdOxModify SnO2Nano composite air-sensitive material and preparation method thereof - Google Patents

More chemical state PdOxModify SnO2Nano composite air-sensitive material and preparation method thereof Download PDF

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CN109110803A
CN109110803A CN201810878833.6A CN201810878833A CN109110803A CN 109110803 A CN109110803 A CN 109110803A CN 201810878833 A CN201810878833 A CN 201810878833A CN 109110803 A CN109110803 A CN 109110803A
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pdo
chemical state
sensitive material
composite air
nano composite
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CN109110803B (en
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齐天骄
杨希
左继
杨芳
闫凡凡
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
    • C01G55/004—Oxides; Hydroxides
    • 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • 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
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • 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 more chemical state PdOxModify SnO2Nano composite air-sensitive material and preparation method, comprising the following steps: palladium chloride is dissolved in ethanol solution, prepares precursor solution；A certain amount of stannic oxide nano powder, sodium borohydride and palladium chloride solution are weighed, is added sequentially in deionized water, then magnetic agitation is taken out reactant, filter, be dried after repeatedly washing, obtain more chemical state PdOxModify SnO2Precursor material；Gained precursor material is placed in Muffle furnace, is calcined in air atmosphere, obtains that there are more chemical state PdOxModify SnO2Nano composite air-sensitive material.The present invention does not generate poisonous and harmful substance, is conducive to environmental protection；Gas sensitive obtained is to H2Show higher sensitivity and selectivity.

Description

More chemical state PdOxModify SnO2Nano composite air-sensitive material and preparation method thereof
Technical field
The present invention relates to gas sensitive technical fields, and in particular to a kind of more chemical state PdOxModify SnO2Nano combined gas Quick material and preparation method thereof.
Background technique
Hydrogen as reducibility gas and carrier gas be widely used to aerospace, auto manufacturing, semiconductor production and The fields such as chemical；Meanwhile hydrogen also results in the very big concern of people, but hydrogen molecule as pollution-free clean energy resource It is small, it is easily revealed in production, transmission and use process, meeting open fire may explode；And the presence of hydrogen can be to metal Generate damage.Currently, research is a kind of short-cut method for realizing hydrogen real-time detection to the response sensitive material of hydrogen, it can be right Hydrogen content in air and specific environment carries out fast and accurately in situ measurement.
There is many years history with the gas sensitive of metal oxide production sensor.Stannic oxide is typical broad stopband N-type semiconductor, forbidden band width are 3.6eV, but since the material is broad spectrum type gas sensitive, can generate sound to multiple gases It should change, it is not high to the selectivity of gas with various；In addition, the knot between the adsorption potential and binding molecule of tin dioxide gas-sensitive material Close thermal energy that can greatly at room temperature, it is therefore desirable to which the sensitivity and response characteristic just having had at high temperature, factors above constrain Development and application of the tin dioxide material on air-sensitive performance.
Summary of the invention
It is an object of the invention to propose a kind of more chemical state PdOxModify SnO2The preparation side of nano composite air-sensitive material Method, the material can be to H2There is good response characteristic.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of more chemical state PdOxModify SnO2The preparation method of nano composite air-sensitive material is that palladium chloride is dissolved in solvent In, prepare precursor solution；A certain amount of stannic oxide nano powder, sodium borohydride and palladium chloride solution are weighed, successively It is add to deionized water, then magnetic agitation is taken out reactant, filter, be dried after repeatedly washing, and obtains polyvoltine Learn state PdOxModify SnO2Precursor material；Gained precursor material is placed in Muffle furnace, is calcined in air atmosphere, is obtained With more chemical state PdOxModify SnO2Nano composite air-sensitive material；
The specific steps of which are as follows:
(1) palladium chloride is dissolved in solvent, obtains precursor solution；
(2) precursor solution that stannic oxide nano powder, sodium borohydride and step (1) obtain is sequentially added into deionization In water, magnetic agitation makes its fully reacting, filters, and is repeatedly dried after washing, obtains PdOxModify SnO2Precursor material；
(3) persursor material that step (2) obtains is placed in Muffle furnace, is forged at a certain temperature in air atmosphere A period of time is burnt, more chemical state PdO are obtainedxModify SnO2Nano composite air-sensitive material.
Further, the quality volume of stannic oxide nano powder described in step (2), sodium borohydride, precursor solution Than for (250~350) mg:(15~30) mg:(8~12) mL.
Further, the stannic oxide nano powder, sodium borohydride, precursor solution mass volume ratio be 300mg:20mg:10mL
Further, solvent described in step (1) be ethyl alcohol or deionized water any one.
Further, precursor solution concentration described in step (1) is from 0.75wt%~10wt%.
Further, tin oxide nano particles granularity described in step (2) is 50~70nm.
Further, magnetic agitation speed described in step (2) is 350~500r/min.
Further, drying described in step (2) refers to dries in the baking oven that temperature is 80~100 DEG C.
Further, calcination temperature is set described in step (3) as 100~700 DEG C.
Further, calcination time is set as 1~2h described in step (3).
Further, the control calcining heating rate in step (3) is 2~10 DEG C/min until reaching set temperature.
The present invention also provides a kind of more chemical state PdOxModify SnO2Nano composite air-sensitive material is provided by the present invention More chemical state PdOxModify SnO2What the preparation method of nano composite air-sensitive material was prepared.
The invention has the following beneficial effects: (1), the present invention by control calcination temperature and calcination time, obtains difference The PdO of chemical statex, different chemical state PdOxModify SnO2Spatial activity site is different, and the adsorption and de-adsorption of gas is also not Together, by adjusting different chemical state PdOx(Pd2+、Pd4+Deng) ratio, can be improved gas response sensitivity, increase stability； (2) the more chemical state PdO of the invention obtainedxModify SnO2Material is to H2It shows higher sensitivity and quick response is restored, detection Limit low, selectivity height, for H2Detection provides a kind of effective sensitive material；(3) gas sensitive structure produced by the present invention and Preparation process is simple, and one step of preparation process is completed, and effectively improves material preparation efficiency, each step during the preparation process is not Poisonous and harmful substance is generated, environmental protection is conducive to.
Detailed description of the invention
Fig. 1 is more chemical state PdO prepared by embodiment 1xModify SnO2Nano composite air-sensitive material STEM-EDS figure；
Fig. 2 is more chemical state PdOx modification SnO2 nano composite air-sensitive material TEM high-resolution contrast item prepared by embodiment 1 Line figure；
Fig. 3 is more chemical state PdO prepared by embodiment 1xModify SnO2Nano composite air-sensitive material Pd3d5/2With O1s XPS Figure；
Fig. 4 is more chemical state PdO prepared by embodiment 1xModify SnO2Nano composite air-sensitive material is 100ppm's to concentration H2The dynamic response recovery curve of gas；
Fig. 5 is more chemical state PdO prepared by embodiment 1xModify SnO2Nano composite air-sensitive material is to various concentration H2Gas Dynamic response recovery curve, linear relationship and its long-time stability；
Fig. 6 is more chemical state PdO prepared by embodiment 1xModify SnO2Other gas of the nano composite air-sensitive material to 100ppm The remolding sensitivity of body compared with.
Specific embodiment
Following further describes the present invention with reference to the drawings.
Embodiment 1
5mg palladium chloride is dissolved in 100mL ethanol solution, PdCl is prepared2Solution；Weigh the stannic oxide of 300mg Nano-powder, 20mg sodium borohydride and 10mL 5wt%PdOxCl2, sequentially add in 100mL deionized water, magnetic agitation 2h, take out Filter, is dried after repeatedly washing, obtains more chemical state PdOxModify SnO2Precursor material；Gained precursor material is set In Muffle furnace, 450 DEG C of calcinings in air atmosphere, heating rate is 5 DEG C/min, keeps temperature 2h, is naturally cooling to room temperature, Obtain that there are more chemical state PdOxModify SnO2Nano composite air-sensitive material.At 80 DEG C, the H for being 100ppm to concentration2Resistance is rung Should rate be 250.
The more chemical state PdO being preparedxModify SnO2Nano composite air-sensitive material STEM-EDS figure is as shown in Fig. 1, by Fig. 1 can be seen that in SnO2Area load PdOx；Fig. 2 is more chemical state PdOxModify SnO2Nano composite air-sensitive material position is brilliant Lattice bar graph can determine the interplanar distance of its composite material by measuring, to further prove SnO2Surface exists PdOx；Fig. 3 is more chemical state PdO of preparationxModify SnO2Nano composite air-sensitive material Pd3d5/2Scheme with O1s XPS, illustrates SnO2 There are the PdO of different chemical states on surfacexElement is；More chemical state PdOxModify SnO2Nano composite air-sensitive material is to concentration The H of 100ppm2The dynamic response recovery curve of gas is as shown in Fig. 4, illustrates the material to H2There is preferable response characteristic, spirit Sensitivity reaches 250；Fig. 5 illustrates more chemical state PdOxModify SnO2H of the nano composite air-sensitive material to various concentration2Response is in Existing stepped change, with H2Concentration increases, and response changing sensitivity increases, linear fit R2=0.999；Fig. 6 illustrates chemistry State PdOxModify SnO2Nano composite air-sensitive material is to H2With highly selective.
Embodiment 2
0.75mg palladium chloride is dissolved in 100mL ethanol solution, PdCl is prepared2Solution；Weigh the titanium dioxide of 300mg Tin nano-powder, 20mg sodium borohydride and 10mL 0.75wt%PdOxCl2, sequentially add in 100mL deionized water, magnetic agitation 2h is filtered, is dried after repeatedly washing, obtains more chemical state PdOxModify SnO2Precursor material；By gained predecessor material Material is placed in Muffle furnace, in air atmosphere 120 DEG C of calcinings, and heating rate is 5 DEG C/min, is kept temperature 1h, is naturally cooling to Room temperature obtains having more chemical state PdOxModify SnO2Nano composite air-sensitive material.At 80 DEG C, the H for being 100ppm to concentration2 Electrical response rate is 7.8.
Embodiment 3
5mg palladium chloride is dissolved in 100mL ethanol solution, PdCl is prepared2Solution；Weigh the stannic oxide of 300mg Nano-powder, 20mg sodium borohydride and 10mL 5wt%PdOxCl2, sequentially add in 100mL deionized water, magnetic agitation 2h, take out Filter, is dried after repeatedly washing, obtains more chemical state PdOxModify SnO2Precursor material；Gained precursor material is set In Muffle furnace, 250 DEG C of calcinings in air atmosphere, heating rate is 5 DEG C/min, keeps temperature 2h, is naturally cooling to room temperature, Obtain that there are more chemical state PdOxModify SnO2Nano composite air-sensitive material.At 80 DEG C, the H for being 100ppm to concentration2Resistance is rung Should rate be 98.
Embodiment 4
(1)H2Measurement: by adjust heating voltage, control the operating temperature of gas sensitive at 80 DEG C, using constant potential Method, in the case where loop voltage keeps 1V constant, the change in electric by recording gas sensitive device obtains gas sensitive in sky Resistance variations in gas and under test gas；
(2) response of gas sensitive are as follows: S=Ra/Rg, wherein RaFor the aerial resistance of sensor, RgFor sensor Resistance under test gas；
(3) use Devince By Dynamic Gas Ration Method by H2Calibrating gas, concentration 500ppm are passed through gas test platform, by gas Sensor component is exposed under test gas, dilutes H using mass flowmenter (MFC) or high-precision air distribution system2Calibrating gas, Its response is measured, 100ppmH is obtained2Change curve is responded, as shown in Figure 3.Using mass flow controller prepare 2.5~ 100ppm ethyl alcohol calibrating gas, is passed through gas test platform, gas sensitive is exposed under test gas, measures its response, Ethanol concentration gradient curve is obtained, as shown in Figure 4.Same procedure is used simultaneously, prepares 100ppmH2、CO、CH4、CH3CH2OH's Calibrating gas obtains the gas sensitive device to H2The selectivity of gas, as a result as shown in figure 5, the gas sensor is to low concentration H2Have good Good response sensitivity, and there is strong interference ability.
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, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application Within scope and spirit.

Claims (10)

1. a kind of more chemical state PdOxModify SnO2The preparation method of nano composite air-sensitive material, which is characterized in that including following Palladium chloride: (1) being dissolved in solvent by step, obtains precursor solution；(2) by stannic oxide nano powder, sodium borohydride and step Suddenly the precursor solution that (1) obtains sequentially adds in deionized water, and magnetic agitation makes its fully reacting, filters, repeatedly after washing It is dried, obtains PdOxModify SnO2Precursor material；(3) persursor material that step (2) obtains is placed in Muffle furnace In, calcining for a period of time, obtains more chemical state PdO at a certain temperature in air atmospherexModify SnO2Nano composite air-sensitive material Material.
2. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is, stannic oxide nano powder described in step (2), sodium borohydride, precursor solution mass volume ratio be (250~ 350) mg:(15~30) mg:(8~12) mL.
3. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is, solvent described in step (1) be ethyl alcohol or deionized water any one.
4. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that precursor solution concentration described in step (1) is 0.75wt%~10wt%.
5. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that stannic oxide nano powder granularity described in step (2) is 50~70nm.
6. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that magnetic agitation speed described in step (2) is 350~500r/min.
7. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that drying described in step (2) refers to dries in the baking oven that temperature is 80~100 DEG C.
8. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that calcination temperature described in step (3) is 100~700 DEG C, and calcination time is 1~2h.
9. more chemical state PdO according to claim 1xModify SnO2The preparation method of nano composite air-sensitive material, it is special Sign is that it is 2~10 DEG C/min until reaching set temperature that the calcining in step (3), which also needs to control calcining heating rate,.
10. a kind of more chemical state PdOxModify SnO2Nano composite air-sensitive material, which is characterized in that more chemical state PdOxIt repairs Adorn SnO2Nano composite air-sensitive material is that the preparation method as described in claim 1~9 any one claim is prepared 's.
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CN112924498A (en) * 2021-01-22 2021-06-08 华中科技大学 Palladium monoatomic modified tin oxide composite material and preparation method and application thereof
CN112924498B (en) * 2021-01-22 2022-04-01 华中科技大学 Palladium monoatomic modified tin oxide composite material and preparation method and application thereof

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