CN107686125A - A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive - Google Patents

A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive Download PDF

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CN107686125A
CN107686125A CN201710758015.8A CN201710758015A CN107686125A CN 107686125 A CN107686125 A CN 107686125A CN 201710758015 A CN201710758015 A CN 201710758015A CN 107686125 A CN107686125 A CN 107686125A
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gas sensitive
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graded structure
sns
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CN107686125B (en
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郝娟媛
张健
张一健
孙权
郑晟良
王铀
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Heilongjiang Industrial Technology Research Institute Asset Management Co ltd
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

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Abstract

A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive.The invention belongs to gas sensitive field, and in particular to a kind of Al adulterates flower-shaped graded structure SnS2The preparation method of gas sensitive.The invention aims to solve existing to be based on inorganic two-dimensional layer SnS2The NO of nano material2Sensor is unable to the problem of working and room temperature.Method：Using stannic chloride pentahydrate as tin source, thiocarbamide is sulphur source, and ANN aluminium nitrate nonahydrate is silicon source, and using ethylene glycol as solvent, the method heated by a step microwave synthesizes the flower-shaped graded structure SnS of Al doping2.Al produced by the present invention is adulterated into flower-shaped graded structure SnS2Gas sensor is made, the gas sensor can detect the other NO of ppb concentration levels at room temperature2, high sensitivity, safe and portable, have broad application prospects.

Description

A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive
Technical field
The invention belongs to gas sensitive field, and in particular to a kind of Al doping graded structure stannic disulfide gas sensitive Preparation method.
Background technology
Nitrogen dioxide (NO2) to be that caused one kind is common during industrial fuel burning and automotive emission poisonous have One of the main reason for evil gas is generation acid rain and initiation photochemical fog, except being polluted to environment, it also threatens The health of the mankind, when its concentration is more than 1ppm, breathing problem will be triggered and then respiratory system is caused serious harm, because This, to the NO under various environmental conditions2It is significant to carry out real time on-line monitoring.In polytype gas sensor, Semiconductor transducer receives much concern because possessing the advantages that cost is low, method is easy, device volume is small, can integrate.And semiconductor The core component of gas sensor is Semiconductor gas sensors material, therefore, designs and prepares new half with efficient air-sensitive performance Conductor material is significant to the performance for improving gas sensor.
Stannic disulfide (SnS2) it is a kind of two-dimension nano materials with class graphene-structured, while there is larger ratio table Area and stronger electronegativity, because to NO2Gas has preferably selectivity and higher sensitivity and causes researcher Concern, but at present pure SnS2Gas sensor also need to work (ACS Nano, 2015,9,10313.) at 120 DEG C, Although existing method can reduce operating temperature while transducer sensitivity is improved, sensor still needs to the work at 80 DEG C Make, cause biosensor power consumption higher, prepare complexity, and the side effect of heated current may cause element itself is caused to be lost, Therefore development can working and room temperature based on SnS2Gas sensor it is significant.
The content of the invention
The present invention is to solve existing to be based on inorganic two-dimensional layer SnS2The NO of nano material2Sensor is unable to room temperature work The problem of making, and a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive is provided.
A kind of preparation method of Al doping graded structure stannic disulfide gas sensitive of the present invention is carried out according to the following steps：
First, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, treats that stannic chloride pentahydrate is molten Xie Hou, mixed solution is obtained, add thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation into mixed solution under the conditions of electromagnetic agitation Reaction solution is obtained after 10min~40min；The mol ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5 ~4)：(0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
2nd, the reaction solution for obtaining step 1 is fitted into microwave tube, is reacted under conditions of being 170 DEG C~190 DEG C in temperature Centrifuged after 10min~30min, centrifugation products therefrom first using ethanol clean 3~5 times, then using deionized water cleaning 3~ 5 times, vacuum drying chamber drying is put into, finally gives Al doping graded structures SnS2Gas sensitive.
Beneficial effects of the present invention：
1st, the present invention is prepared for Al doping graded structures SnS using a step microwave method2Gas sensitive, by regulating and controlling nine water Close the controllable graded structure SnS of amount that aluminum nitrate adds2Conductive capability, realize room temperature NO2Response.
2nd, Al adulterates graded structure SnS2Gas sensitive, maintaining SnS2While graded structure, due to mixing for Al Enter, improve based on graded structure SnS2The sensitivity of material gas sensor, at room temperature, the Al obtained using the present invention Adulterate graded structure SnS2Gas sensor prepared by gas sensitive is to 2ppm NO2Sensitivity be 5.4.
Brief description of the drawings
Fig. 1 is that the Al that embodiment one obtains adulterates graded structure SnS2The scanning electron microscope (SEM) photograph of gas sensitive；
Fig. 2 is the graded structure SnS of different Al doping contents2X ray diffracting spectrum, a is pure SnS2Powder；b、c、d Respectively 2%, 3%, and the graded structure SnS of 4%Al doping2；
Fig. 3 is pure SnS2High resolution transmission electron microscopy；
Fig. 4 is that the Al that embodiment one obtains adulterates graded structure SnS2The high resolution transmission electron microscopy of gas sensitive Figure；
Fig. 5 is that the Al obtained using embodiment one adulterates graded structure SnS2Gas sensitive is at room temperature to various concentrations NO2Response -- recovery curve；
Fig. 6 is that the Al obtained using embodiment one adulterates graded structure SnS2Gas sensitive at room temperature sensitivity with NO2 The relation curve of change in concentration.
Embodiment
Embodiment one：A kind of preparation of Al doping graded structure stannic disulfide gas sensitives of present embodiment Method is carried out according to the following steps：
First, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, treats that stannic chloride pentahydrate is molten Xie Hou, mixed solution is obtained, add thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation into mixed solution under the conditions of electromagnetic agitation Reaction solution is obtained after 10min~40min；The mol ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5 ~4)：(0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
2nd, the reaction solution for obtaining step 1 is fitted into microwave tube, is reacted under conditions of being 170 DEG C~190 DEG C in temperature Centrifuged after 10min~30min, centrifugation products therefrom first using ethanol clean 3~5 times, then using deionized water cleaning 3~ 5 times, vacuum drying chamber drying is put into, finally gives Al doping graded structures SnS2Gas sensitive.
Embodiment two：Present embodiment is unlike embodiment one：Five water four described in step 1 The mol ratio of stannic chloride, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.03.Other steps and parameter and the phase of embodiment one Together.
Embodiment three：Present embodiment is unlike embodiment one or two：Five described in step 1 The mol ratio of water butter of tin, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.05.Other steps and parameter and embodiment One or two is identical.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Institute in step 1 The concentration for stating stannic chloride pentahydrate in mixed solution is 0.1mol/L.Other steps and parameter and embodiment one to three it One is identical.
Embodiment five：Unlike one of present embodiment and embodiment one to four：In step 2 Temperature is reacted under conditions of being 180 DEG C.Other steps and parameter are identical with one of embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：It is anti-in step 2 Centrifuged after answering 20min.Other steps and parameter are identical with one of embodiment one to five.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of Al doping graded structures SnS2The preparation method of gas sensitive is carried out according to the following steps：
First, 0.3156g stannic chloride pentahydrates are added in 15mL ethylene glycol solutions under conditions of electromagnetic agitation, treat five Mixed solution is obtained after the dissolving of water butter of tin, adds 0.1370g thiocarbamides and 270 into mixed solution under the conditions of electromagnetic agitation The ethylene glycol solution (concentration 0.1mol/L) of μ L ANN aluminium nitrate nonahydrates, magnetic agitation 20min obtain reaction solution；
2nd, the reaction solution for obtaining step 1 is fitted into microwave tube, after reacting 20min under conditions of being 180 DEG C in temperature Centrifuge, centrifugation products therefrom is first cleaned 3~5 times using ethanol, then is cleaned 3~5 times using deionized water, is put into vacuum and is done Dry case is dried, and obtains Al doping graded structures SnS2The doping of gas sensitive, wherein Al is 3%.
3%Al doping graded structures SnS is obtained using the method for embodiment one2Gas sensitive, its scanning electron microscope (SEM) photograph is such as Shown in Fig. 1, it can be seen that Al adulterates SnS2Graded structure is by SnS2The flower-like structure of nanometer sheet composition.The XRD spectrums of the material Figure is as shown in curve c in Fig. 2, with pure SnS2Compared to (the SnS of curve a), Al doping2XRD spectra in (001) crystal face diffraction Peak is offset to low angle direction, mainly due to the incorporation of Al atoms so that and (001) interplanar distance becomes big, and other crystal faces Peak position does not almost move, but the remitted its fury at peak, also further illustrates that Al incorporation causes SnS2Crystallinity die down. HRTEM tests the doping for having also further demonstrated that Al atoms, and Fig. 3 is pure SnS2HRTEM pictures, (001) interplanar distance is 0.587nm；And Al adulterates SnS in Fig. 42HRTEM pictures in, (001) interplanar distance is 0.642nm, illustrates Al incorporation only (001) interplanar distance is set to become big.
By the SnS of Al doping graded structures2Gas sensitive is dissolved in ethanol, is configured to 10mg/mL solution, ultrasound After 10min, Al doping SnS is obtained2Dispersion liquid, Al is adulterated by SnS by the method for instillation2Dispersant liquid drop to electrode slice surface, 1h, after alcohol solvent volatilization, the SnS of Al doping are dried under conditions of being 70 DEG C in temperature2It is homogeneous by being formed in electrode surface Film, the electrode slice are used directly for air-sensitive performance test.
Air-sensitive performance is tested by electrochemical workstation, the sensitivity S of sensor is defined as：S=Rg/Ra, wherein RaTo pass The aerial resistance of sensor, RgIt is sensor in NO2In resistance value.Its test result as shown in figure 5, test result shows, At room temperature, the Al obtained using embodiment one adulterates the SnS of graded structure2Gas sensor prepared by gas sensitive is being inhaled Attached NO2After gas, the resistance value of sensor can significantly increase, and with NO2Concentration is increasing, and the sensitivity of sensor is also bright Aobvious increase, in NO2Sensitivity when concentration is 2ppm is 5.4, and pure SnS2, can not at room temperature because conductive capability is poor It is used as sensor.Fig. 6 is the SnS that the Al obtained using embodiment one adulterates graded structure2Air-sensitive prepared by gas sensitive passes The response sensitivity of sensor is with NO2The relation curve of change in concentration, NO2Concentration between 0.25~6ppm, transducer sensitivity with NO2The approximate linear change of concentration.
Embodiment two：The present embodiment and the difference of embodiment one are：Stannic chloride pentahydrate described in step 1 Quality is 3.156g, and the quality of thiocarbamide is 1.370g, the ethylene glycol solution (concentration 0.1mol/L) of ANN aluminium nitrate nonahydrate 2.7mL.Other steps and parameter are identical with embodiment one.
Embodiment three：The present embodiment is with the difference of embodiment one：The second of ANN aluminium nitrate nonahydrate is added in step 1 The μ L of glycol solution (concentration 0.1mol/L) 90.Other steps and parameter are identical with embodiment one.
Example IV：The present embodiment is with the difference of embodiment one：The second of ANN aluminium nitrate nonahydrate is added in step 1 The μ L of glycol solution (concentration 0.1mol/L) 450.Other steps and parameter are identical with embodiment one.
Embodiment five：The present embodiment is with the difference of embodiment one：In step 2 under conditions of temperature is 190 DEG C Centrifuged after reaction 10min.Other steps and parameter are identical with embodiment one.
Embodiment six：The present embodiment is with the difference of embodiment one：In step 2 under conditions of temperature is 170 DEG C Centrifuged after reaction 30min.Other steps and parameter are identical with embodiment one.
The Al doping graded structures SnS that the present embodiment is obtained using embodiment one2Gas sensing prepared by gas sensitive Device, which solves, existing is based on pure SnS2Gas sensor the problem of being unable to working and room temperature, and Al doping SnS2Sensor is in room temperature Lower to have higher sensitivity, this improves SnS mainly due to the doping of Al atoms2Conductive capability, while increase point Hierarchical organization SnS2The gas absorption avtive spot on gas sensitive surface.

Claims (6)

  1. A kind of 1. preparation method of Al doping graded structure stannic disulfide gas sensitive, it is characterised in that Al doping graduation knots The preparation method of structure stannic disulfide gas sensitive is carried out according to the following steps：
    First, stannic chloride pentahydrate is added in ethylene glycol solution under the conditions of electromagnetic agitation, after stannic chloride pentahydrate dissolving, Mixed solution is obtained, adds thiocarbamide and ANN aluminium nitrate nonahydrate, magnetic agitation 10min into mixed solution under the conditions of electromagnetic agitation Reaction solution is obtained after~40min；The mol ratio of the stannic chloride pentahydrate, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:(1.5~4)： (0.01~0.05), the concentration of stannic chloride pentahydrate is 0.03~0.6mol/L in the mixed solution；
    2nd, the reaction solution for obtaining step 1 is fitted into microwave tube, reacts 10min under conditions of being 170 DEG C~190 DEG C in temperature Being centrifuged after~30min, centrifugation products therefrom is first cleaned 3~5 times using ethanol, then is cleaned 3~5 times using deionized water, Vacuum drying chamber drying is put into, finally gives Al doping graded structures SnS2Gas sensitive.
  2. 2. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, it is special Sign is that the mol ratio of stannic chloride pentahydrate described in step 1, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.03.
  3. 3. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, it is special Sign is that the mol ratio of stannic chloride pentahydrate described in step 1, thiocarbamide and ANN aluminium nitrate nonahydrate is 1:2:0.05.
  4. 4. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, it is special Sign concentration of stannic chloride pentahydrate in the mixed solution described in step 1 is 0.1mol/L.
  5. 5. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, it is special Sign is reacted under conditions of being 180 DEG C in temperature in step 2.
  6. 6. a kind of preparation method of Al doping graded structure stannic disulfide gas sensitive according to claim 1, it is special Sign centrifuges after 20min is reacted in step 2.
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Cited By (5)

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CN108562615A (en) * 2018-01-02 2018-09-21 潘远新 A kind of nitrogen dioxide leakage detector of working and room temperature
CN109211985A (en) * 2018-09-01 2019-01-15 哈尔滨工程大学 A kind of flexibility alkaline gas sensing chip and preparation method thereof
CN110095506A (en) * 2019-04-04 2019-08-06 海南聚能科技创新研究院有限公司 Au/SnS2Nitrogen dioxide gas sensor and preparation process and application
CN112578001A (en) * 2019-09-30 2021-03-30 天津大学 Gas sensitive material based on Zn-doped stannous sulfide, preparation method thereof and application thereof in methanol detection
CN114646669A (en) * 2022-03-16 2022-06-21 哈尔滨工业大学 Preparation method and application of tin disulfide/tin diselenide transverse heterostructure gas-sensitive material

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108562615A (en) * 2018-01-02 2018-09-21 潘远新 A kind of nitrogen dioxide leakage detector of working and room temperature
CN109211985A (en) * 2018-09-01 2019-01-15 哈尔滨工程大学 A kind of flexibility alkaline gas sensing chip and preparation method thereof
CN109211985B (en) * 2018-09-01 2020-12-04 哈尔滨工程大学 Flexible alkaline gas sensing chip and preparation method thereof
CN110095506A (en) * 2019-04-04 2019-08-06 海南聚能科技创新研究院有限公司 Au/SnS2Nitrogen dioxide gas sensor and preparation process and application
CN112578001A (en) * 2019-09-30 2021-03-30 天津大学 Gas sensitive material based on Zn-doped stannous sulfide, preparation method thereof and application thereof in methanol detection
CN112578001B (en) * 2019-09-30 2021-12-21 天津大学 Gas sensitive material based on Zn-doped stannous sulfide, preparation method thereof and application thereof in methanol detection
CN114646669A (en) * 2022-03-16 2022-06-21 哈尔滨工业大学 Preparation method and application of tin disulfide/tin diselenide transverse heterostructure gas-sensitive material
CN114646669B (en) * 2022-03-16 2024-05-28 哈尔滨工业大学 Preparation method and application of tin disulfide/tin diselenide transverse heterostructure gas-sensitive material

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