CN106946283B - 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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CN106946283B
CN106946283B CN201710202237.1A CN201710202237A CN106946283B CN 106946283 B CN106946283 B CN 106946283B CN 201710202237 A CN201710202237 A CN 201710202237A CN 106946283 B CN106946283 B CN 106946283B
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composite material
tinbase
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sno
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CN106946283A (en
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胡杰
王莹
王影
王文达
薛炎
李朋伟
李刚
连崑
张文栋
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Taiyuan University of Technology
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    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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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 light concentration gas non sensitivity be present 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,Sodium hydroxide,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,High sensitivity,Fast response time,Suitable low concentration acetone detection,It can be applied in acetone gas sensor is detected,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 are quick Feel the technical field that material is prepared and applied.
Background technology
Acetone has been used widely in industrial circle as a kind of chemical reagent, such as：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； Caused by breathing in hundreds of metabolin, acetone is related to diabetes, the acetone concentration that normal person breathes out 0.3-0.9ppm it Between, and the acetone concentration of diabetes patient's exhalation is in more than 1.8ppm, how precisely rapidly to detect acetone is ten to human health Divide important.
Generally, acetone gas is detected using gas chromatography and mass spectrometry, but used in these technologies Equipment takes up an area big, complex operation；Metal semiconductor oxide gas sensor detector due to make easily, detection it is accurate, be Detect the optimal selection of acetone gas.
At present, metal semiconductor oxide gas sensor is also in research, there is many deficiencies, for example, pure phase is golden Category conductor oxidate mostly exist sensitivity is low, response speed is slow, selectivity and stability are 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 shortcomings that being directed to current gas detection technology and deficiency, using adding nitre in stannous chloride Sour praseodymium, reacted kettle Hydrothermal Synthesiss, vacuum heat, the tinbase nano composite material for detecting acetone is made, to increase substantially 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 uses is：Stannous chloride, praseodymium nitrate, sodium citrate, sodium hydroxide, anhydrous second Alcohol, deionized water, oxygen, nitrogen, it is as follows that it combines preparation dosage：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, sodium hydroxide 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, ultrasonic disperse, ultrasonic frequency are carried out 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. opening micro-injection pump, speed 1mL/min, 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, it is 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 During heating, Hydrothermal Synthesiss redox reaction will occur 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. stopping heating after Hydrothermal Synthesiss, 23 DEG C are naturally cooled to；
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 ethyl alcohol wash, centrifuge
By in the centrifuge tube equipped with sediment, deionized water 50mL is added, is centrifuged, centrifuge revolution 7000r/ Min, time 5min is centrifuged, upper liquid is discarded after separation；
Absolute ethyl alcohol 50mL is added in centrifuge tube, is shaken up, centrifuge revolution 7000r/min, centrifuges time 5min, Sediment is retained after separation, discards upper liquid；
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 microwave heating, oxygen transfer, Completed under nitrogen guard mode；
1. Tin Composite Material is laid in silica crucible, microwave oven middle part is subsequently placed in, and it is closed；
2. opening nitrogen cylinder, 20% oxygen, the mixed gas of 80% nitrogen are inputted into microwave oven, mixed gas Input speed 200cm3/ min, make in stove invariablenes pressure of liquid in 0.1MP a；
Open outlet pipe valve simultaneously, pressure and constant in regulating stove；
3. opening the microwave applicator of calcining furnace, 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 with 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 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 It is kept 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 have with background technology compared with it is obvious advanced, be for acetone gas detect gas sensitive exist it is 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, Sodium hydroxide, 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, and up to 99%, material is sensitive to 100ppm acetone air-sensitives Degree, to the sensitivity of 1ppm acetone gas up to 1.86, high sensitivity, responds up to 27, response time 2s, recovery time 36s 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, microwave heating 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 vacuumize, oxygen transfer+ Completed under nitrogen, microwave heating, the cooling of outer water circulation；
Vacuum microwave sintering furnace 1 is vertical, and in the bottom of vacuum microwave sintering furnace 1 be electric cabinet 2, top is bell 3, 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 be 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, microwave heating 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 measuring coordinate curve map of acetone, and for material to acetone high sensitivity, response resume speed is fast, right 100ppm acetone Gas-sensing measurment is up to 27, response time 2s, recovery time 36s；It is to 1 and 5ppm acetone gas to scheme medium and small figure The measuring coordinate curve magnification figure of body, to the sensitivity of 1ppm acetone gas up to 1.86, to low concentration acetone high sensitivity, 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 1. 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, sodium hydroxide, absolute ethyl alcohol, deionized water, Oxygen, nitrogen, it is as follows that it combines preparation dosage：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. weighing stannous chloride 9g ± 0.001g, sodium citrate 29.4g ± 0.001g, sodium hydroxide 1.6g ± 0.001g, add 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, ultrasonic disperse is carried out, ultrasonic frequency 50kHz, is added 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. opening micro-injection pump, speed 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, it is 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 Redox reaction will occur 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. stopping heating after Hydrothermal Synthesiss, 23 DEG C are naturally cooled to；
    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 centrifuges, centrifuge revolution 7000r/min, centrifuges time 10min, sediment, abandoning supernatant are retained after separation；
    8. deionized water, absolute ethyl alcohol wash, centrifuge
    By in the centrifuge tube equipped with sediment, deionized water 50mL is added, is centrifuged, centrifuge revolution 7000r/min, Time 5min is centrifuged, upper liquid is discarded after separation；
    Absolute ethyl alcohol 50mL is added in centrifuge tube, is shaken up, centrifuge revolution 7000r/min, centrifuges time 5min, separation 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 microwave heating, oxygen transfer, nitrogen Completed under guard mode；
    1. Tin Composite Material is laid in silica crucible, microwave oven middle part is subsequently placed in, and it is closed；
    2. opening nitrogen cylinder, 20% oxygen, the mixed gas of 80% nitrogen, the input of mixed gas are inputted into microwave oven Speed 200cm3/ min, make in stove invariablenes pressure of liquid in 0.1MPa；
    Open outlet pipe valve simultaneously, pressure and constant in regulating stove；
    3. opening the microwave applicator of calcining furnace, 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/SnO2Color and luster, pattern, Chemical Physics performance, the air-sensitive performance of nano composite material 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. 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 vacuumize, oxygen transfer+nitrogen Completed under gas, microwave heating, the cooling of outer water circulation；
    Vacuum microwave sintering furnace (1) to be vertical, in the bottom of vacuum microwave sintering furnace (1) be electric cabinet (2), top be bell (3), inside 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；Sintered in vacuum microwave The right lower quadrant of stove (1) is provided with vavuum pump (10), and vavuum pump (10) top is provided with vacuum valve (11), vacuum tube (12), vacuum meter (13), and with furnace chamber (9) connect；Nitrogen cylinder (14), oxygen cylinder (17), nitrogen are provided with side by side in the left part of vacuum sintering furnace (1) Bottle (14) top is provided with nitrogen tube (15), nitrogen valve (16) and connects gas mixing pipe (20)；Set on oxygen cylinder (17) top There are oxygen hose (18), oxygen valve (19), and connect mixture pipe (20)；Mixture pipe (20) top is provided with gaseous mixture body surface (21), and connect furnace chamber (9) and mixed gas (22) is inputted into furnace chamber (9)；Mixed gas (22) is by 20% oxygen+80% Nitrogen forms；Display screen (24), indicator lamp (25), power switch (26), controller for vacuum pump are provided with electric cabinet (2) (27), microwave heating controller (28).
CN201710202237.1A 2017-03-30 2017-03-30 A kind of preparation method for the tinbase nano composite material for detecting low concentration acetone gas Active CN106946283B (en)

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