CN106946283A - A kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas - Google Patents

A kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas Download PDF

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CN106946283A
CN106946283A CN201710202237.1A CN201710202237A CN106946283A CN 106946283 A CN106946283 A CN 106946283A CN 201710202237 A CN201710202237 A CN 201710202237A CN 106946283 A CN106946283 A CN 106946283A
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composite material
tinbase
nano composite
gas
sno
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CN106946283B (en
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胡杰
王莹
王影
王文达
薛炎
李明伟
李刚
连崑
张文栋
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Taiyuan University of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00Compounds of tin
    • C01G19/02Oxides
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating 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
    • G01N27/125Composition of the body, e.g. the composition of its sensitive layer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/50Agglomerated particles
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The present invention relates to a kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas, it is there is light concentration gas non sensitivity for acetone gas detection gas sensitive, high concentrations of gas sensitivity is low, response speed is slow, select the situation of stability difference, with stannous chloride, NaOH, sodium citrate, praseodymium nitrate is raw material, reacted kettle Hydrothermal Synthesiss, microwave heating high-temperature is heat-treated, grinding sieving, obtain tinbase nano composite material, this preparation method technique is advanced, data are accurately full and accurate, product morphology is good, for the flower-shaped hierarchy of piece shape, piece thickness≤30nm, product purity is good, up to 99%, material is to 100ppm acetone Gas-sensing measurment up to 27, response time is 2s, recovery time is 36s, to 1ppm acetone gas sensitivity up to 1.86, sensitivity is high, fast response time, suitable low concentration acetone detection, it can be applied in detection acetone gas sensor, it is the preparation method of advanced tinbase nano composite material.

Description

A kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas
Technical field
The present invention relates to a kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas, category gas is quick Feel the technical field that material is prepared and applied.
Background technology
Acetone is used widely in industrial circle as a kind of chemical reagent, for example:Purify paraffin, dissolving plastics and Rubber, synthesis chloroform and epoxy resin, produce organic hyaline monomer etc.;But contact and suction acetone can cause nausea, fatigue, head Bitterly, vomit, even go into a coma;In addition, acetone or human body metabolite, its concentration can reflect human body state; Breathe produce hundreds of metabolin in, acetone is related to diabetes, normal person breathe out acetone concentration 0.3-0.9ppm it Between, and how the acetone concentration of diabetes patient's exhalation precisely rapidly detects that acetone is ten to human health in more than 1.8ppm Divide important.
Generally, acetone gas is detected using gas chromatography and mass spectrometry, but used by these technologies Equipment takes up an area big, complex operation;Metal semiconductor oxide gas sensor detector is accurate due to making easy, detection, is Detect the optimal selection of acetone gas.
At present, metal semiconductor oxide gas sensor is many not enough also in research, also having, for example, pure phase is golden Category conductor oxidate mostly has that sensitivity is low, response speed slow, selectivity and stability it is poor, to low concentration under test gas without The shortcomings of sensitivity, it is difficult to meet the complicated requirement of gas sensor in actual applications;In order to improve the spirit of gas sensor Sensitivity, response speed, directional selectivity, meet application request, the often doping load agent in gas sensitive, or by different Matter knot is to strengthen the gas-sensitive property of gas sensitive, and technique is also in conceptual phase.
The content of the invention
Goal of the invention
The purpose of the present invention is the shortcoming and defect for current gas detection technology, using adding nitre in stannous chloride Sour praseodymium, the tinbase nano composite material of detection acetone is made, to increase substantially in reacted kettle Hydrothermal Synthesiss, vacuum heat Sensitivity, stability and the response speed of gas sensitive, so as to improve detection performance in gas sensor application.
Technical scheme
The chemical substance material that the present invention is used is:Stannous chloride, praseodymium nitrate, sodium citrate, NaOH, anhydrous second Alcohol, deionized water, oxygen, nitrogen, it is as follows that it combines preparation consumption:With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) selected chemical substance material
Preparing the chemical substance material that uses will carry out selected, and carry out quality purity control:
(2) praseodymium nitrate ethanol solution is prepared
Weigh praseodymium nitrate 1g ± 0.001g to add in beaker, measure absolute ethyl alcohol 10mL ± 0.001mL, add in beaker, Stirring and dissolving 10min, into 0.23mol/L praseodymium nitrate ethanol solution;
(3) tinbase Pr is prepared6O11/Sn3O4/SnO2Nano composite material
Tinbase Pr6O11/Sn3O4/SnO2The preparation of nano composite material is carried out in heating furnace, reactor, is to add Completed during heat, Hydrothermal Synthesiss;
1. stannous chloride 9g ± 0.001g, sodium citrate 29.4g ± 0.001g, NaOH 1.6g ± 0.001g are weighed, Add in beaker;
Absolute ethyl alcohol 200mL ± 0.001mL, deionized water 300mL ± 0.001mL are measured, is added in beaker, it is molten into mixing Liquid;
2. the beaker for filling mixed solution is placed in ultrasonic wave separating apparatus, carries out ultrasonic disperse, ultrasonic frequency 50kHz, 30 DEG C of heating-up temperature, ultrasonic disperse time 20min, into transparent mixed solution;
3. after ultrasonic disperse, transparent mixed solution is transferred on magnetic stirring apparatus and stirred;
4. micro-injection pump is opened, speed is 1mL/min, and the praseodymium nitrate of preparation is instilled into the beaker for fill mixed solution Ethanol solution 10mL ± 0.001mL, and 10min is stirred, into transparent mixed solution;
5. the transparent mixed solution prepared is moved into polytetrafluoroethylcontainer container, be subsequently placed in reactor, and it is closed;
Reactor is placed in heating furnace and heated, 200 DEG C ± 2 DEG C of heating-up temperature, heat time 480min;Transparent mixing is molten Redox reaction will occur during heating, Hydrothermal Synthesiss for liquid, and reaction equation is as follows:
In formula:Sn(OH)2:Stannous hydroxide, SnO:Stannous oxide, SnO2:Tin oxide, Pr (OH)3:Praseodymium hydroxide, NaCl:Sodium chloride, C6H8O7:Citric acid;
6. stop heating after Hydrothermal Synthesiss, naturally cool to 23 DEG C;
7. centrifuge
Reactor in heating furnace is taken out, the mixed solution in polytetrafluoroethylcontainer container is placed in centrifugal separating tube with suction pipe In, it is centrifuged, centrifuge revolution 7000r/min, centrifuges time 10min, retain sediment after separation, discard Clear liquid;
8. deionized water, absolute ethanol washing, are centrifuged
In the centrifuge tube that will be equipped with sediment, deionized water 50mL is added, is centrifuged, centrifuge revolution 7000r/ Min, centrifuges time 5min, upper liquid is discarded after separation;
Absolute ethyl alcohol 50mL is added in centrifuge tube, is shaken up, centrifuge revolution 7000r/min, time 5min is centrifuged, Sediment is retained after separation, upper liquid is discarded;
Deionized water, washes of absolute alcohol are used respectively 5 times, centrifugation repeats 5 times respectively;
9. it is dried in vacuo
Sediment after cleaning is placed in quartz container, is then placed in vacuum drying chamber and dries, 70 DEG C of drying temperature, Vacuum 2Pa, drying time 360min, into Tin Composite Material;
(4) Tin Composite Material is heat-treated
The heat treatment of dried Tin Composite Material is carried out in microwave oven, be heating using microwave, oxygen transfer, Completed under nitrogen guard mode;
1. Tin Composite Material is laid in silica crucible, is subsequently placed in microwave oven middle part, and it is closed;
2. nitrogen cylinder is opened, 20% oxygen, the mixed gas of 80% nitrogen are inputted into microwave oven, mixed gas Input speed 200cm3/ min, makes in stove invariablenes pressure of liquid in 0.1Mpa;
Outlet pipe valve is opened simultaneously, pressure and constant in regulating stove;
3. the microwave applicator of calcining furnace is opened, 3 DEG C/min of the rate of heat addition is raised to 500 DEG C ± 2 DEG C of temperature, and in the temperature Lower holding 120min;
In heat treatment process, by the Pr generated in hydro-thermal reaction (OH)3Decompose, reaction equation is as follows:
In formula:Pr6O11:Praseodymium oxide, Sn3O4:Four three tin of oxidation, SnO2:Tin oxide, H2O:Vapor;
After heat treatment, into end-product tinbase Pr6O11/Sn3O4/SnO2Nano composite material;
(5) grind, sieve
By tinbase Pr6O11/Sn3O4/SnO2Nano composite material grinds 10min in ball mill, then uses 650 eye mesh screens Sieving, grinding, sieving repeat;
Into end-product tinbase Pr after grinding, sieving6O11/Sn3O4/SnO2Flower-shaped fine powder;
(6) test, analysis and characterization
To the tinbase Pr of preparation6O11/Sn3O4/SnO2The color and luster of nano composite material, pattern, Chemical Physics performance, air-sensitive Performance carries out test, analysis and characterization;
Morphology analysis is carried out with Electronic Speculum;
Matter Composition analysis is carried out with XRD analysis instrument;
Gas-sensitive property analysis is carried out to acetone gas with intelligent air-sensitive measuring and analysing meter;
Conclusion:Tinbase Pr6O11/Sn3O4/SnO2Nano composite material be the flower-shaped hierarchy of piece shape, piece thickness≤30nm, Product purity is up to 99%;
(7) product storage
The tinbase Pr of preparation6O11/Sn3O4/SnO2Nano composite material is stored in the glass container of amber transparent, closed Keep in dark place, moistureproof, sun-proof, anti-acid-alkali salt corrodes, 22 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has obvious advanced with background technology compared with, is that to detect that gas sensitive is present for acetone gas low Concentration gases non sensitivity, high concentrations of gas sensitivity are low, response speed is slow, the situation of selection stability difference, with stannous chloride, NaOH, sodium citrate, praseodymium nitrate are raw material, and reacted kettle Hydrothermal Synthesiss, microwave heating high-temperature heat treatment, grinding are sieved, Obtain tinbase Pr6O11/Sn3O4/SnO2Nano composite material, this preparation method technique is advanced, and data are accurately full and accurate, product morphology It is good, it is the flower-shaped hierarchy of piece shape, piece thickness≤30nm, product purity is good, up to 99%, material is sensitive to 100ppm acetone air-sensitives Degree is up to 27, and the response time is 2s, and recovery time is 36s, and to the sensitivity of 1ppm acetone gas up to 1.86, sensitivity is high, response Resume speed is fast, suitable low concentration acetone detection, can be applied in the sensor of detection acetone gas, be advanced tinbase Pr6O11/Sn3O4/SnO2The preparation method of nano composite material.
Brief description of the drawings
Fig. 1, tinbase Pr6O11/Sn3O4/SnO2Nano composite material condition of heat treatment figure;
Fig. 2, tinbase Pr6O11/Sn3O4/SnO2Nano composite material shape appearance figure;
Fig. 3, tinbase Pr6O11/Sn3O4/SnO2Nano composite material X-ray diffraction intensity collection of illustrative plates;
Fig. 4, tinbase Pr6O11/Sn3O4/SnO2Nano composite material air-sensitive performance figure;
Shown in figure, list of numerals is as follows:
1st, microwave agglomerating furnace, 2, electric cabinet, 3, bell, 4, workbench, 5, quartz container, 6, tinbase nano composite material, 7th, container silk screen, 8, microwave applicator, 9, furnace chamber, 10, vavuum pump, 11, vacuum valve, 12, vacuum tube, 13, vacuum meter, 14, nitrogen Gas cylinder, 15, nitrogen tube, 16, nitrogen valve, 17, oxygen cylinder, 18, oxygen hose, 19, oxygen valve, 20, gas mixing pipe, 21, mixing Gas meter, 22, mixed gas, 23, outlet pipe valve, 24, display screen, 25, indicator lamp, 26, power switch, 27, vavuum pump control Device, 28, heating using microwave controller, 29, outer water circulation cooling tube, 30, water intaking valve, 31, outlet valve, 32, wire.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
It is tinbase Pr shown in Fig. 16O11/Sn3O4/SnO2Nano composite material condition of heat treatment figure, each portion position is correct, Match, sequentially operate according to quantity;
The value for preparing the chemical substance used is determined by the scope pre-set, with gram, milliliter, centimetre3For meter Measure unit.
The heat treatment of tinbase nano composite material is carried out in vacuum microwave sintering furnace, be vacuumizing, oxygen transfer+ Completed under nitrogen, heating using microwave, the cooling of outer water circulation;
Vacuum microwave sintering furnace 1 to be vertical, be in the bottom of vacuum microwave sintering furnace 1 electric cabinet 2, top be bell 3, it is interior Portion is furnace chamber 9;Workbench 4 is provided with the inner bottom part of furnace chamber 9, quartz container 5 is put on the top of workbench 4, built in quartz container 5 Tinbase nano composite material 6 is put, is covered on the top of quartz container 5 by container silk screen 7;On the inwall of vacuum microwave sintering furnace 1 Provided with microwave applicator 8;Outer water circulation cooling tube 29, water intaking valve 30, water outlet are arranged with the external rings of vacuum microwave sintering furnace 1 Valve 31, and be connected with external water source;Vavuum pump 10 is provided with the right lower quadrant of vacuum microwave sintering furnace 1, the top of vavuum pump 10 is provided with Vacuum valve 11, vacuum tube 12, vacuum meter 13, and connected with furnace chamber 9;Vacuum sintering furnace 1 left part side by side provided with nitrogen cylinder 14, Oxygen cylinder 17, the top of nitrogen cylinder 14 is provided with nitrogen tube 15, nitrogen valve 16 and connects gas mixing pipe 20, on the top of oxygen cylinder 17 Provided with oxygen hose 18, oxygen valve 19, and mixture pipe 20 is connected, the top of mixture pipe 20 is provided with gaseous mixture body surface 21, and connects Furnace chamber 9 simultaneously inputs mixed gas 22 into furnace chamber 9, and mixed gas 22 is made up of the nitrogen of 20% oxygen+80%;On electric cabinet 2 Provided with display screen 24, indicator lamp 25, power switch 26, controller for vacuum pump 27, heating using microwave controller 28.
It is tinbase Pr shown in Fig. 26O11/Sn3O4/SnO2The shape appearance figure of nano composite material, shown in figure, composite is The flower-shaped hierarchy of piece shape, piece thickness≤30nm.
It is tinbase Pr shown in Fig. 36O11/Sn3O4/SnO2Nano composite material X-ray diffraction intensity collection of illustrative plates, shown in figure, Ordinate is diffracted intensity, and abscissa is the θ of the angle of diffraction 2, symbol ◆ be Sn3O4Diffraction maximum, symbolFor Pr6O11Diffraction maximum, Remaining is SnO2Diffraction maximum.
It is tinbase Pr shown in Fig. 46O11/Sn3O4/SnO2Nano composite material air-sensitive performance figure, shown in figure, big figure is tin Based nano composite material is to the measurement coordinate curve of acetone, and material is to acetone sensitivity height, and response resume speed is fast, right 100ppm acetone Gas-sensing measurment is up to 27, and the response time is 2s, and recovery time is 36s;It is to 1 and 5ppm acetone gas to scheme medium and small figure The measurement coordinate curve enlarged drawing of body, it is high to the sensitivity of low concentration acetone to the sensitivity of 1ppm acetone gas up to 1.86, it can expire Demand in the gas sensor of the actually detected acetone of foot;
Gas-sensing measurment:The resistance value in resistance value/acetone gas in air.

Claims (2)

1. a kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas, it is characterised in that:
The chemical substance material used is:Stannous chloride, praseodymium nitrate, sodium citrate, NaOH, absolute ethyl alcohol, deionized water, Oxygen, nitrogen, it is as follows that it combines preparation consumption:With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) selected chemical substance material
Preparing the chemical substance material that uses will carry out selected, and carry out quality purity control:
(2) praseodymium nitrate ethanol solution is prepared
Weigh praseodymium nitrate 1g ± 0.001g to add in beaker, measure absolute ethyl alcohol 10mL ± 0.001mL, add in beaker, stirring 10min is dissolved, into 0.23mol/L praseodymium nitrate ethanol solution;
(3) tinbase Pr is prepared6O11/Sn3O4/SnO2Nano composite material
Tinbase Pr6O11/Sn3O4/SnO2The preparation of nano composite material is carried out in heating furnace, reactor, be heating, Completed during Hydrothermal Synthesiss;
1. stannous chloride 9g ± 0.001g, sodium citrate 29.4g ± 0.001g, NaOH 1.6g ± 0.001g are weighed, is added In beaker;
Absolute ethyl alcohol 200mL ± 0.001mL, deionized water 300mL ± 0.001mL are measured, is added in beaker, into mixed solution;
2. the beaker for filling mixed solution is placed in ultrasonic wave separating apparatus, progress ultrasonic disperse, ultrasonic frequency 50kHz, plus Hot 30 DEG C of temperature, ultrasonic disperse time 20min, into transparent mixed solution;
3. after ultrasonic disperse, transparent mixed solution is transferred on magnetic stirring apparatus and stirred;
4. micro-injection pump is opened, speed is 1mL/min, the praseodymium nitrate ethanol of preparation is instilled into the beaker for fill mixed solution Solution 10mL ± 0.001mL, and 10min is stirred, into transparent mixed solution;
5. the transparent mixed solution prepared is moved into polytetrafluoroethylcontainer container, be subsequently placed in reactor, and it is closed;
Reactor is placed in heating furnace and heated, 200 DEG C ± 2 DEG C of heating-up temperature, heat time 480min;Transparent mixed solution exists To occur redox reaction during heating, Hydrothermal Synthesiss, reaction equation is as follows:
In formula:Sn(OH)2:Stannous hydroxide, SnO:Stannous oxide, SnO2:Tin oxide, Pr (OH)3:Praseodymium hydroxide, NaCl:Chlorine Change sodium, C6H8O7:Citric acid;
6. stop heating after Hydrothermal Synthesiss, naturally cool to 23 DEG C;
7. centrifuge
Reactor in heating furnace is taken out, the mixed solution in polytetrafluoroethylcontainer container is placed in centrifugal separating tube with suction pipe, entered Row is centrifuged, centrifuge revolution 7000r/min, centrifuges time 10min, sediment, abandoning supernatant are retained after separation;
8. deionized water, absolute ethanol washing, are centrifuged
In the centrifuge tube that will be equipped with sediment, deionized water 50mL is added, is centrifuged, centrifuge revolution 7000r/min, Centrifugation time 5min, upper liquid is discarded after separation;
Absolute ethyl alcohol 50mL is added in centrifuge tube, is shaken up, centrifuge revolution 7000r/min, time 5min, separation is centrifuged After retain sediment, discard upper liquid;
Deionized water, washes of absolute alcohol are used respectively 5 times, centrifugation repeats 5 times;
9. it is dried in vacuo
Sediment after cleaning is placed in quartz container, is then placed in vacuum drying chamber and dries, 70 DEG C of drying temperature, vacuum 2Pa, drying time 360min are spent, into Tin Composite Material;
(4) Tin Composite Material is heat-treated
Dried Tin Composite Material heat treatment is carried out in microwave oven, is in heating using microwave, oxygen transfer, nitrogen Completed under guard mode;
1. Tin Composite Material is laid in silica crucible, is subsequently placed in microwave oven middle part, and it is closed;
2. nitrogen cylinder is opened, 20% oxygen, the mixed gas of 80% nitrogen, the input of mixed gas are inputted into microwave oven Speed 200cm3/ min, makes in stove invariablenes pressure of liquid in 0.1Mpa;
Outlet pipe valve is opened simultaneously, pressure and constant in regulating stove;
3. the microwave applicator of calcining furnace is opened, 3 DEG C/min of the rate of heat addition is raised to 500 DEG C ± 2 DEG C of temperature, and protects at such a temperature Hold 120min;
In heat treatment process, by the Pr generated in hydro-thermal reaction (OH)3Decompose, reaction equation is as follows:
In formula:Pr6O11:Praseodymium oxide, Sn3O4:Four three tin of oxidation, SnO2:Tin oxide, H2O:Vapor;
After heat treatment, into end-product tinbase Pr6O11/Sn3O4/SnO2Nano composite material;
(5) grind, sieve
By tinbase Pr6O11/Sn3O4/SnO2Nano composite material grinds 10min in ball mill, is then sieved with 650 eye mesh screens, Grinding, sieving repeat;
Into end-product tinbase Pr after grinding, sieving6O11/Sn3O4/SnO2Flower-shaped fine powder;
(6) test, analysis and characterization
To the tinbase Pr of preparation6O11/Sn3O4/SnO2The color and luster of nano composite material, pattern, Chemical Physics performance, air-sensitive performance Carry out test, analysis and characterization;
Morphology analysis is carried out with Electronic Speculum;
Matter Composition analysis is carried out with XRD analysis instrument;
Gas-sensitive property analysis is carried out to acetone gas with intelligent air-sensitive measuring and analysing meter;
Conclusion:Tinbase Pr6O11/Sn3O4/SnO2Nano composite material is the flower-shaped hierarchy of piece shape, piece thickness≤30nm, product Purity is up to 99%;
(7) product storage
The tinbase Pr of preparation6O11/Sn3O4/SnO2Nano composite material is stored in the glass container of amber transparent, closed lucifuge Preserve, moistureproof, sun-proof, anti-acid-alkali salt corrodes, 22 DEG C of storage temperature, relative humidity≤10%.
2. a kind of preparation method of tinbase nano composite material for detecting low concentration acetone gas according to claim 1, It is characterized in that:
The heat treatment of tinbase nano composite material is carried out in vacuum microwave sintering furnace, be vacuumizing, oxygen transfer+nitrogen Completed under gas, heating using microwave, the cooling of outer water circulation;
Vacuum microwave sintering furnace (1) is that electric cabinet (2), top are bell in the bottom of vacuum microwave sintering furnace (1) to be vertical (3), internal is furnace chamber (9);Workbench (4) is provided with furnace chamber (9) inner bottom part, quartz container is put on workbench (4) top (5) tinbase nano composite material (6), is put in quartz container (5), is covered on quartz container (5) top by container silk screen (7) Lid;Microwave applicator (8) is provided with the inwall of vacuum microwave sintering furnace (1);Vacuum microwave sintering furnace (1) external rings around Provided with outer water circulation cooling tube (29), water intaking valve (30), outlet valve (31), and it is connected with external water source;In vacuum microwave sintering The right lower quadrant of stove 1 be provided with vavuum pump (10), vavuum pump (10) top be provided with vacuum valve (11), vacuum tube 12, vacuum meter 13, and with Furnace chamber 9 is connected;Nitrogen cylinder 14, oxygen cylinder 17 are provided with side by side in the left part of vacuum sintering furnace 1, and the top of nitrogen cylinder 14 is provided with nitrogen tube 15th, nitrogen valve 16 and gas mixing pipe 20 is connected;Oxygen hose 18, oxygen valve 19 are provided with the top of oxygen cylinder 17, and connects mixing Tracheae 20;The top of mixture pipe 20 is provided with gaseous mixture body surface 21, and connects furnace chamber 9 and mixed gas 22 is inputted into furnace chamber 9; Mixed gas (22) is made up of the nitrogen of 20% oxygen+80%;Display screen 24, indicator lamp 25, power switch are provided with electric cabinet 2 26th, controller for vacuum pump (27), heating using microwave controller (28).
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CN107445196A (en) * 2017-05-25 2017-12-08 南京工业大学 A kind of stratiform Sn3O4/SnO2The preparation method of hetero-junctions square piece type gas sensitive
CN109655499A (en) * 2019-01-23 2019-04-19 中物院成都科学技术发展中心 A kind of gas sensitive and preparation method thereof for nitrogen dioxide sensor
CN111998584A (en) * 2020-08-21 2020-11-27 阜阳九珍食品有限公司 Cooling arrangement is used in production of efficient seasoning
CN113281383A (en) * 2021-05-24 2021-08-20 安徽大学绿色产业创新研究院 Ethanol gas sensor made of heterojunction composite material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105665734A (en) * 2016-01-06 2016-06-15 太原理工大学 Preparation method for gold-loaded tin oxide nanometer material for detecting hydrogen
CN105712405A (en) * 2016-01-06 2016-06-29 太原理工大学 Preparation method of molybdenum-doped tungsten oxide gas-sensitive material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105665734A (en) * 2016-01-06 2016-06-15 太原理工大学 Preparation method for gold-loaded tin oxide nanometer material for detecting hydrogen
CN105712405A (en) * 2016-01-06 2016-06-29 太原理工大学 Preparation method of molybdenum-doped tungsten oxide gas-sensitive material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107445196A (en) * 2017-05-25 2017-12-08 南京工业大学 A kind of stratiform Sn3O4/SnO2The preparation method of hetero-junctions square piece type gas sensitive
CN109655499A (en) * 2019-01-23 2019-04-19 中物院成都科学技术发展中心 A kind of gas sensitive and preparation method thereof for nitrogen dioxide sensor
CN109655499B (en) * 2019-01-23 2021-06-15 中物院成都科学技术发展中心 Gas-sensitive material for nitrogen dioxide sensor and preparation method thereof
CN111998584A (en) * 2020-08-21 2020-11-27 阜阳九珍食品有限公司 Cooling arrangement is used in production of efficient seasoning
CN113281383A (en) * 2021-05-24 2021-08-20 安徽大学绿色产业创新研究院 Ethanol gas sensor made of heterojunction composite material and preparation method thereof
CN113281383B (en) * 2021-05-24 2024-04-12 安徽大学绿色产业创新研究院 Ethanol gas sensor of heterojunction composite material and preparation method thereof

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