CN110376252A - A kind of SnO2The preparation method of nano-powder and transparent gas sensor - Google Patents
A kind of SnO2The preparation method of nano-powder and transparent gas sensor Download PDFInfo
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 75
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000001354 calcination Methods 0.000 claims abstract description 42
- 150000003839 salts Chemical class 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 9
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 230000002378 acidificating effect Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 229910001868 water Inorganic materials 0.000 claims description 14
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 11
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical group Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000002103 nanocoating Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 125000004185 ester group Chemical group 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 17
- 235000019441 ethanol Nutrition 0.000 abstract description 15
- 239000002086 nanomaterial Substances 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract description 10
- 230000004044 response Effects 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 62
- 239000000243 solution Substances 0.000 description 14
- 230000035945 sensitivity Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000001119 stannous chloride Substances 0.000 description 2
- 235000011150 stannous chloride Nutrition 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- DAFHKNAQFPVRKR-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylpropanoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)C DAFHKNAQFPVRKR-UHFFFAOYSA-N 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 244000131316 Panax pseudoginseng Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000021186 dishes Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present invention relates to nano material and transparent gas sensor technical fields more particularly to solution direct oxidation method to prepare SnO2Nano-powder, with pink salt, that is, SnCl of two kinds of different valence states4·5H2O and SnCl2·2H2O is raw material, uses H2O replaces ethyl alcohol as solvent, and acetic acid is stabilizer, prepared SnO at 75-500 DEG C of research2The crystal property and air-sensitive performance of nano-powder establish the realistic model that calcination temperature and Sn chemical valence have otherwise impact to air-sensitive performance, and a kind of pair of alcohol gas of design and assembly has the transparent gas sensor of good air-sensitive response performance.The powder preparation method is simple, product is easy to get, is at low cost, is SnO2The novel transparent sensor for providing certain theoretical direction when nano material is used as gas sensitive, and developing has the characteristics that highly sensitive and fast response time, is conducive to promote and apply in production and living.
Description
Technical field
The present invention relates to nano material and gas sensor technical fields, in particular to be novel solutions direct oxidation method
Preparation has highly sensitive air-sensitive performance SnO2The method of nano material and transparent gas sensor.
Background technique
As a kind of n-type semiconductor (Eg=3.6eV), SnO2Because it has, low cost, physics and chemical property are stable, add
The convenient and simple feature of work, it is considered to be a kind of up-and-coming metal oxide semiconductor material, and it is widely used in gas
The fields such as sensor, lithium ion battery, supercapacitor, solar battery.SnO2Have at a lower temperature to reducibility gas
Very high reactivity, is easy to adsorption of oxygen, works as SnO2After reaching nm rank, material has very high specific surface area and generates quantum
Dimensional effect, it is helpful to the air-sensitive performance for improving gas sensor.SnO2The particle size of powder, the shape of particle, uniformly
Property, stability all directly affect made of the sensitivity of gas sensitive device, power consumption, the response important ginseng such as recovery characteristics and stability
Number.In early days it is believed that after noble metal addition, in SnO2Grain surface, which forms metal cluster, can produce additional absorption position,
On its surface catalytic oxidation-reduction effect occurs for gas.However, polycrystalline SnO2It is increasingly complex with the mechanism of action of reducing gas.
It includes: SnO2The losing of Lattice Oxygen, the modification of tin oxidation state and between intrinsic metal and doping metals new keys shape
At.Currently, commonly synthesizing SnO2The method of nano material mainly has chemical vapour deposition technique, sol-gal process, hydro-thermal method etc..
Choi, U-Sung et al. are by SnO2、Co3O4A series of powders pass through mechanical ball mill for 24 hours, the composite nano-powder being heat-treated
In CO, H2Etc. show good N-shaped respondent behavior (Choi, U-Sung etc., Sensors and in reducing atmospheres
Actuators B:Chemical, 2004,98:166)；Neftali et al. uses organic polymer Sn (OR)4As forerunner's system
It is standby mixed with rare earth element ce, the tin oxide ultra-fine grain of Y, La, partial size 20nm, and there is excellent air-sensitive performance
(Carreno, Neftali LV etc., Journal of Nanoparticle Research, 2009,11:955)；Wang Huan is new etc.
People prepares pure SnO using Hydrolyze method2Nano material optimizes synthesis condition by orthogonal experiment, and compared constant temperature hydrolysis with
The characteristics of microwave hydrolysis, tests gas-sensitive property using static volumetric method, the results showed that, it can be obtained uniformly with Microwave Water solution
Tiny SnO2Nano material greatly shortens the time of synthetic reaction, and the reactant concentration of plastic increases, and production efficiency is obvious
Improve (Wang Huan is new etc., Journal of Rare Earths, 2010,28:171).The key problem in technology of conventional sol gel method is
The technology of preparing of colloidal sol is mostly used SnCl4Aqueous solution is as predecessor.But the type of initial feed salt, calcination temperature, SnO2's
The correlative study that structure etc. influences air-sensitive performance needs further perfect, solves SnO with this2Base gas sensor stability
The disadvantages of difference, selectivity is bad.
Summary of the invention
The object of the invention is that being improved to solve the above-mentioned problems and in original preparation method, propose
A kind of novel solution direct oxidation process, to improve SnO2The air-sensitive performance of nano material.
The present invention is through the following technical solutions to achieve the above objectives: a kind of SnO of high sensitivity2The preparation of nano-powder
Method carries out the preparation of presoma using the pink salt of two kinds of different valence states, i.e., that choose respectively is SnCl4·5H2O and SnCl2·
2H2O is prepared by novel solutions direct oxidation method, is included the following steps:
(1) acetic acid is added to the water, obtains acidic aqueous solution；
The volume ratio of acetic acid and water is 25:150-350, preferably 25:270 in the acidic aqueous solution；
(2) under stirring, in the step of mixed solution of pink salt and acetic acid is slowly dropped to 30 DEG C of constant temperature (1)
To acidic aqueous solution in, after being added dropwise, continue to stir 2-6h, after still aging 72-120h, obtain SnO2Colloidal sol；
The pink salt is SnCl4·5H2O or SnCl2·2H2O；Pink salt in the mixed solution of the pink salt and acetic acid
Proportionate relationship with acetic acid is 0.1mol:20-40mL, preferably 0.1mol:30mL；The mixed solution of the pink salt and acetic acid
Volume with acidic aqueous solution is 4.375-18.75:1, preferably 9.83:1；
(3) by SnO obtained in step (2)2Colloidal sol is in 75-500 DEG C (such as 75 DEG C, 250 DEG C, 500 DEG C) calcining 2-40h
(such as 40h, 15h, 2h), obtains SnO2Nano-powder.
Preferably, the acetic acid could alternatively be hydrochloric acid or nitric acid；When the hydrochloric acid or nitric acid, dosage is acetic acid
The 1/6-1/8 of volume.
Preferably, the revolving speed of the stirring is 100-600r/min.
Preferably, described to be slowly added dropwise to be added dropwise dropwise, such as 5-10mL/min.
The invention further relates to the SnO of Sustainable use method as described above preparation2Nano-powder, average particle size range are
3.42nm-22.42nm。
The present invention also provides a kind of transparent gas sensors, utilize SnO described above2Nano-powder preparation.
The preparation method of transparent gas sensor described above, includes the following steps:
(1) by prepared SnO2Nano material is mixed with water, is added coalescing agent, is prepared into slurry；
(2) slurry that step (1) obtains is coated uniformly on glass carrier, after dry, obtains SnO2Nano coating
(3) SnO obtained in step (2)2The surface of nano coating applies Ag electrode, is prepared into transparent gas sensor.
Wherein: SnO2Nano-powder: water: the mass ratio of coalescing agent is 1:1-2:0.05-0.2；SnO2The area of coating with
The proportionate relationship of slurry is 5-20cm2: 1g.
Preferably, the temperature of the drying is 250 DEG C, and the dry time is 1-3h；
Preferably, the coalescing agent is ester alcohol 12.
Preferably, the glass carrier is silica glass carrier.
Preferably, the present invention is that the coating shape of this Ag electrode is designed as trident by the electrical efficiency of increase Ag electrode
Type.
In above-mentioned clear sensor structure, it is based on SnO2The gas sensor of material is under different operating temperatures to not
Same reducibility gas (such as carbon monoxide, ethyl alcohol, nitrogen dioxide) has different susceptibilitys, therefore is applicable to local environment
The detection of middle pernicious gas.But the shadow due to the resistance of sensor by working environment (temperature, humidity and other gases)
It rings, especially directly-heated type gas sensor, sensitive and heating element thermal capacitance is all smaller, compares the response speed of gas
Fastly, it is easy to be affected by the ambient temperature.No matter powered using voltage source or current source to heater strip, when environment temperature occurs
When variation, the temperature of heater strip can all change, to affect the Stability and veracity of sensor detection.The present invention uses number
Word PI control, is added to a heating electrode, optimizes the structure of sensor, and holding adding thermal resistance is steady state value, makes sensor
Work is under a stable absolute temperature, to eliminate influence of the variation to sensor of environment temperature.By to ethyl alcohol
The detection of gas and analysis to its experimental result, show the shadow that this method can effectively inhibit environment temperature to gas sensor
It rings.
Preferably, the SnO made from stannous salt2Have when nano material partial size is smaller, calcination temperature is lower more excellent
Good air-sensitive performance；And SnO made from tetravalence pink salt2When nano material partial size is larger, calcination temperature is higher gas sensitivity compared with
It is good；When reducibility gas concentration of alcohol is 500ppm, by using SnCl under 250 DEG C of calcinings2·2H2SnO made from O2Nanometer material
Expect and by using SnCl under 500 DEG C of calcinings4·5H2SnO made from O2The gas sensing response of nano material is best, and is sensed
Resistance ratio of the device in air and object gas is roughly the same, may each be about 3.5, and air-sensitive performance performance at this time is very excellent.Its
Middle sensing response SGIt is defined as the ratio of Ra/Rg, Ra and Rg are respectively resistance of the sensor in air and object gas.
Specifically, the present invention can solution oxide method preparation SnO direct at low temperature2Nano-powder, this method have widened SnO2
The preparation method of nano-powder has very big novelty.
The present invention prepares clear sensor part using the form of small size and film, the mainly SnO utilized2Broadband
Three kinds of features of gap, small size and film, the transparent gas sensor are put forward for the first time, and be expected to enlargement gas sensor uses model
It encloses.
The highest gas sensitivity of the transparent gas sensor has reached 3.5 times, i.e., in detection gas, the electricity of sensor
Resistance rate reduces 1/3.5th that amplitude is original.This illustrates that the transparent gas sensor has reached ideal adaptable journey
Degree, the transparent gas sensor are expected to play very big effect in gas detection occasion.
The utility model has the advantages that
The present invention prepares SnO by novel solutions direct oxidation method2Nano-powder, the pink salt with two kinds of different valence states are
SnCl4·5H2O and SnCl2·2H2O is raw material, uses H2O replaces ethyl alcohol as solvent, and acetic acid is stabilizer, studies 75-500 DEG C
Prepared SnO under (low middle high i.e. 75 DEG C, 250 DEG C, 500 DEG C three different calcination temperatures)2The crystal property of nano-powder is gentle
Quick performance establishes the realistic model that calcination temperature and Sn chemical valence have Different Effects to air-sensitive performance, and design and assembly
A kind of transparent gas sensor, the sensor have good air-sensitive response performance to alcohol gas.Powder preparation method behaviour
To make simply, product is easy to get, and it is at low cost, it is SnO2Certain theoretical direction is provided when nano material is used as gas sensitive,
And the transparent gas sensor newly proposed is conducive to promote and apply in production and living, highest gas sensitivity has reached 3.5
Times, i.e., in detection gas, the resistivity of sensor reduces amplitude is original 1/3.5th, passes through the inspection to alcohol gas
Survey and the analysis to its experimental result show the influence that this method can effectively inhibit environment temperature to gas sensor, therefore develop
Novel transparent sensor out has the characteristics that wide detection range, highly sensitive, high-precision, fast response time and interchangeability are good,
It may insure the accuracy that automated production detects and controls.
Detailed description of the invention
Fig. 1 is SnCl in embodiment 14·5H2The substances such as O make the presoma of raw material preparation, obtain by different calcination temperatures
SnO2The XRD spectrum of nano-powder.
Fig. 2 is SnCl in embodiment 22·2H2The substances such as O make the presoma of raw material preparation, obtain by different calcination temperatures
SnO2The XRD spectrum of nano-powder.
Fig. 3 is transparent gas sensor structure schematic diagram of the present invention；
In figure: 1. heating electrodes, 2.SnO2Nano coating, 3. measuring electrodes, 4.SiO2Glass carrier.
Fig. 4 is SnO2Nano-powder gas sensitivity measuring system；
In figure: 5. magnetic force constent temperature heaters, 6. evaporating dishes, 7. samples (gas sensor), 9. iron stand of 8.1L beaker, 10. note
Emitter, 11. copper wire, 12. multimeters, 9.PET film, 10. thermometers.
Fig. 5 is different ethanol concentration to SnO made from different valence state pink salt under different calcination temperatures2The air-sensitive of nano-powder
Sensing response figure.
Specific embodiment
Following nonlimiting examples can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Embodiment 1
Pink salt SnCl4·5H2O SnO obtained under different calcination temperatures as presoma2Nano-powder, including walk as follows
It is rapid:
(1) it is put into 270ml water in beaker, 25ml acetic acid to solution ph is added and is equal to 2, obtain acidic aqueous solution, 30 DEG C
It is lower to keep stirring this beaker on the magnetic stirring apparatus of 300r/min.
(2) 35.06g stannic chloride pentahydrate (SnCl is weighed4·5H2O, 0.1mol) solid is added in another beaker, then plus
Enter acetic acid 30ml, be allowed to dissolve, obtains the mixed solution of pink salt and acetic acid.
(3) mixed solution of pink salt and acetic acid that step (2) obtains is added drop-wise to the rate stirring with 300r/min dropwise
In the acidic aqueous solution that the step of state (1) obtains, after continuing stirring 2h, still aging 72h after being added dropwise, SnO is obtained2It is molten
Glue.
(4) SnO for obtaining step (3)2Colloidal sol pass through respectively 75 DEG C, 250 DEG C, 500 DEG C and respectively calcine 40h, 15h,
Carefully grinding obtains three parts of SnO after 2h2Nano-powder.The wherein SnO that 75 DEG C of calcining 40h are obtained2Nano-powder is denoted as No.1 SnO2
Nano-powder；The SnO that 250 DEG C of calcining 15h are obtained2Nano-powder is denoted as No. two SnO2Nano-powder, particle size values 4.73nm；
The SnO that 500 DEG C of calcining 2h are obtained2Nano-powder is denoted as No. three SnO2Nano-powder, particle size values 22.42nm.
Fig. 1 is SnCl4·5H2The substances such as O make the presoma of raw material preparation, the SnO obtained by different calcination temperatures2It receives
The XRD spectrum of rice flour body.It will be seen from figure 1 that with Sn4+The raw materials such as pink salt made from dry thermal crystallisation at a temperature of 75 DEG C of colloid
Treated, and nano-powder is undefined structure, does not form SnO2Crystal.It may be due to SnCl under low temperature drying system4It is water-soluble
Moisture evaporation is slower in glue, and the polycondensation reaction rate occurred between sol solutions is slow, and the time for being transformed into gel is long, at this time not
Three strongest peak is occurred, and shows amorphous peak, the colloidal sol nodeless mesh phenomenon.And SnCl4·5H2It is made under the substance reactions system such as O
Sn4+Sample by 250 DEG C and 500 DEG C of calcined powders by with SnO2Standard diagram control, discovery is SnO2Crystal form.
When calcination temperature is 500 DEG C, the peak value of diffraction maximum is more sharp in obtained XRD diagram, illustrates that its crystal property is preferable,
Without other substances generate, and with the lower 250 DEG C of obtained SnO of crystallization temperature2The XRD diagram phase that nano material powder is formed
Than, halfwidth is very narrow, and crystallite dimension is smaller, therefore it follows that when to contain Sn4+Pink salt be raw material made of presoma into
SnO when row calcining, when temperature is higher synthesized by it2Particle diameter of nanometer powder is bigger, and crystal property is more preferable.Mechanism present in it
It may be the easier evaporation of temperature more high-moisture, polycondensation reaction is accelerated, and is more less likely to occur to reunite between particle, so that initially
The SnCl of beginning4Preferably oxidation, and become SnO2The time of gel shortens, and the nucleation of nanoparticle and growth are more preferable at this time, is made
SnO2Nano-powder has grain development complete, the good advantage of crystal property.
Embodiment 2
Pink salt SnCl2·2H2O SnO obtained under different calcination temperatures as presoma2Nano-powder, including walk as follows
It is rapid:
(1) 270ml water is put into beaker, addition 25ml acetic acid is equal to 2 up to solution ph, obtains acidic aqueous solution, will
This beaker is kept stirring on the magnetic stirring apparatus of 300r/min at 30 DEG C.
(2) two hydrate (SnCl of 22.5g stannous chloride is weighed2·2H2O, 0.1mol) solid is added to another beaker
In, acetic acid 30ml is added, is allowed to dissolve, obtains the mixed solution of pink salt and acid.
(3) mixed solution of pink salt and acid that step (2) obtains is added drop-wise to dropwise and shape is stirred with the rate of 300r/min
In the acidic aqueous solution that the step of state (1) obtains, after continuing stirring 2h, still aging 72h after being added dropwise, SnO is obtained2It is molten
Glue.
(4) SnO for obtaining step (3)2Colloidal sol pass through respectively 75 DEG C, 250 DEG C, 500 DEG C and respectively calcine 40h, 15h,
Carefully grinding obtains three parts of SnO after 2h2Nano-powder.The wherein SnO that 75 DEG C of calcining 40h are obtained2Nano-powder is denoted as No. four SnO2
Nano-powder；The SnO that 250 DEG C of calcining 15h are obtained2Nano-powder is denoted as No. five SnO2Nano-powder, particle size values 3.42nm；
The SnO that 500 DEG C of calcining 2h are obtained2Nano-powder is denoted as No. six SnO2Nano-powder, particle size values 18.34nm.
Fig. 2 is SnCl2·2H2The substances such as O make the presoma of raw material preparation, the SnO obtained by different calcination temperatures2It receives
The XRD spectrum of rice flour body.Figure it is seen that with Sn2+The raw materials such as pink salt made from colloid no matter at 75 DEG C, 250 DEG C or
500 DEG C are all crystalline structure, however, it will be apparent that can find out that the three strongest peak of 75 DEG C of calcined nano-powders is different from other two,
The discovery of reference standards map and SnCl2Three strongest peak match, illustrate the SnCl in raw material2Shakiness is not oxidized by oxygen into
Fixed SnO becomes SnO in turn2Crystal.Though calcination temperature three strongest peak occurs when being 250 DEG C, halfwidth is very wide, diffraction maximum
Lower, though illustrating that it has crystallization, crystallinity is bad, and the long-range of atomic arrangement is not so regular, but shortrange order, interior
Portion is there are many amorphous, though atom confusing array, but still actually SnO2Crystal.Contrastingly, when calcination temperature is 500 DEG C
When, the peak value of diffraction maximum is more sharp in obtained XRD diagram, and halfwidth is relatively narrow, illustrates that its crystal property is preferable, without it
He generates substance.Thus it is concluded that, when to contain Sn2+Pink salt be presoma made of raw material when being calcined, temperature compared with
Low SnO synthesized by it2Nano particle diameter is smaller, and performance is more superior.It may be since high temperature is conducive to Sn4+The oxidation of ion
And growth, more, crystallization effect is more preferably for the facilitation effect of nucleation and production to nanoparticle.
Embodiment 3
Pink salt SnCl4·5H2O SnO obtained under different calcination temperatures as presoma2Nano-powder, including walk as follows
It is rapid:
(1) 270ml water is put into beaker, addition 4.17ml hydrochloric acid is equal to 2 up to solution ph, obtains acidic aqueous solution,
This beaker will be kept stirring on the magnetic stirring apparatus of 300r/min at 30 DEG C.
(2) 35.6g stannic chloride pentahydrate (SnCl is weighed4·5H2O) solid is added in another beaker, adds hydrochloric acid
5ml is allowed to dissolve, and obtains the mixed solution of pink salt and hydrochloric acid.
(3) mixed solution of pink salt and hydrochloric acid that step (2) obtains is added drop-wise to the rate stirring with 300r/min dropwise
In the acidic aqueous solution that the step of state (1) obtains, after continuing stirring 2h, still aging 72h after being added dropwise, SnO is obtained2It is molten
Glue.
(4) SnO for obtaining step (3)2Colloidal sol pass through respectively 75 DEG C, 250 DEG C, 500 DEG C and respectively calcine 40h, 15h,
Carefully grinding obtains three parts of SnO after 2h2Nano-powder.The wherein SnO that 75 DEG C of calcining 40h are obtained2Nano-powder is denoted as No. seven SnO2
Nano-powder；The SnO that 250 DEG C of calcining 15h are obtained2Nano-powder is denoted as No. eight SnO2Nano-powder；What 500 DEG C of calcining 2h were obtained
SnO2Nano-powder is denoted as No. nine SnO2Nano-powder.
Embodiment 4
Pink salt SnCl2·2H2O SnO obtained under different calcination temperatures as presoma2Nano-powder, including walk as follows
It is rapid:
(1) 270ml water is put into beaker, addition 3.125ml nitric acid is equal to 2 up to solution ph, obtains acidic aqueous solution,
This beaker will be kept stirring on the magnetic stirring apparatus of 300r/min at 30 DEG C.
(2) two hydrate (SnCl of 22.5g stannous chloride is weighed2·2H2O) solid is added in another beaker, is added
3.75ml nitric acid is allowed to dissolve, and obtains the mixed solution of pink salt and nitric acid.
(3) mixed solution of pink salt and nitric acid that step (2) obtains is added drop-wise to the rate stirring with 300r/min dropwise
In the acidic aqueous solution that the step of state (1) obtains, after continuing stirring 2h, still aging 72h after being added dropwise, SnO is obtained2It is molten
Glue.
(4) SnO for obtaining step (3)2Colloidal sol pass through respectively 75 DEG C, 250 DEG C, 500 DEG C and respectively calcine 40h, 15h,
Carefully grinding obtains three parts of SnO after 2h2Nano-powder.The wherein SnO that 75 DEG C of calcining 40h are obtained2Nano-powder is denoted as No. ten SnO2
Nano-powder；The SnO that 250 DEG C of calcining 15h are obtained2Nano-powder is denoted as ride on Bus No. 11 SnO2Nano-powder；500 DEG C of calcining 2h are obtained
SnO2Nano-powder is denoted as ten No. two SnO2Nano-powder.
Embodiment 5
Respectively by No. two, No. three SnO in embodiment 12No. five, No. six SnO in nano-powder and embodiment 22Nano powder
System is made transparent gas sensor, and wherein the substrate of transparent gas sensor is designed as thin column shape, thickness 2mm, be with
The silica glass of insulation is carrier.The cross circular section radius of substrate is 10mm, and area is about 31.4mm2.Gas sensitive SnO2
It is mixed with deionized water, adds Yi Shiman TEXANOL coalescing agent (ester alcohol 12), be prepared into slurry, this slurry is uniformly coated
On silica glass carrier, drying in drying box is placed it in, again in SnO after taking-up2Nano coating surface applies Ag electrode,
It is prepared into transparent gas sensor.Wherein, SnO2Nano-powder: deionized water: coalescing agent is 1g:2g:0.2g；Dry temperature
250 DEG C of degree, drying time 2h；SnO2The area of coating and the proportionate relationship of slurry are 10cm2: 1g；Measuring electrode and heating electrode
Upper surface of substrate is occupy, electrode material is Ag, and schematic shapes are as shown in figure 3, interdigital distribution there are three measuring electrode bands
In SnO2Material area finally converges at same pin, and uses the test electrode and general-purpose on copper wire connection gas sensor
Table tests the resistance change of gas sensor under various concentration with this.The present invention is controlled using number PI, is added to one
Electrode is heated, optimizes the structure of sensor, holdings adding thermal resistance is steady state value, keeps working sensor stable absolute at one
At a temperature of, to eliminate influence of the variation to sensor of environment temperature.
Embodiment 6
Fig. 4 is SnO2Nano-powder gas sensitivity measuring system, it is transparent to four kinds in embodiment 5 with the measuring system
Gas sensor carries out sensitivity test.The measurement process be one by PET film sealing beaker (volume 1L) in into
It is capable (referring to Liu, S., L.Li, W.Jiang, C.Liu, W.Ding, and W.Chai.Crystallinity and
morphology-controlled synthesis of SnO2nanoparticles for higher gas
Sensitivity.Powder Technology, 2013 (245): 168-173.), and sample (SnO is mounted in instrument2Gas
Quick element), evaporating dish and thermometer.Temperature in measurement beaker is controlled by magnetic force constent temperature heater and is accurately monitored with thermometer
Temperature change in measurement process, to guarantee SnO2Constant film temperature is 150 DEG C.When measurement, with the syringe of 1mL by ethyl alcohol
It is injected into the evaporating dish for measurement, forms alcohol vapour at 150 DEG C.Ethanol vapor concentration be respectively 100ppm,
200ppm, 300ppm, 400ppm, 500ppm and with multimeter to SnO2The change in resistance of gas sensor carry out real-time monitoring and
Record, so that resistance variations data are analyzed.Sensor responds SGIt is defined as Ra/Rg ratio, wherein Ra and Rg is respectively to pass
Sensor is exposed to the resistance before and after alcohol vapour.
Measurement result is as shown in figure 5, using stannous salt as SnO made of raw material under 250 DEG C of calcination temperatures2Nano-powder
Air-sensitive performance is better than powder obtained at higher temperature i.e. 500 DEG C, and is made under 500 DEG C of calcination temperatures using tetravalence pink salt by raw material
SnO2The gas sensitivity of nano-powder is better, the powder obtained at 250 DEG C better than this presoma.This is because SnO2
The factors such as the air-sensitive performance of nano-powder and crystal form, particle size and crystallinity are related, so working as institute under same calcination temperature
When the raw material tin ion valence state difference of use, the biggish gas sensitivity of difference can be also shown.In view of this when tin in pink salt
When the valence state of ion is divalent, the nano-powder air-sensitive performance that calcination temperature is lower, size of microcrystal is small is good；When stanniferous ion raw material
Valence state when being tetravalence, the nano-powder air-sensitive performance that calcination temperature is high, size of microcrystal is big is good.As shown in Figure 4,250 DEG C of calcinings
At a temperature of using stannous salt as SnO made of raw material2It is made under nano-powder and 500 DEG C of calcination temperatures using tetravalence pink salt by raw material
SnO2The air-sensitive performance highest of nano-powder, the sensitivity of the two has all reached 3.5 times, i.e., in detection gas, two kinds of biographies
The resistivity of sensor reduces 1/3.5th that amplitude is original, divides by the detection to alcohol gas and to its experimental result
Analysis, shows the influence that this method can effectively inhibit environment temperature to gas sensor.
For any person skilled in the art, without departing from the scope of the technical proposal of the invention, all
Many possible changes and modifications are made to technical solution of the present invention using the technology contents of the disclosure above, or are revised as equivalent
The equivalent embodiment of variation.Therefore, anything that does not depart from the technical scheme of the invention, according to the technical essence of the invention to
Any simple modifications, equivalents, and modifications that upper embodiment is done should all still fall within the range of technical solution of the present invention protection
It is interior.
Claims (10)
1. a kind of SnO2The preparation method of nano-powder, characterized by the following steps:
(1) acetic acid is added to the water, obtains acidic aqueous solution；
The volume ratio of acetic acid and water is 25:150-350 in the acidic aqueous solution；
(2) under stirring, obtained in the step of mixed solution of pink salt and acetic acid is slowly dropped to 30 DEG C of constant temperature (1)
In acidic aqueous solution, after being added dropwise, continues to stir 2-6h, after standing 72-120h, obtain SnO2Colloidal sol；
The pink salt is SnCl4·5H2O or SnCl2·2H2O；Pink salt and acetic acid in the mixed solution of the pink salt and acetic acid
Proportionate relationship be 0.1mol:20-40mL；The mixed solution of pink salt and acetic acid and the volume of acidic aqueous solution be
4.375-18.75:1；
(3) by SnO obtained in step (2)2Colloidal sol obtains SnO in 75-500 DEG C of calcining 2-40h2Nano-powder.
2. SnO according to claim 12The preparation method of nano-powder, it is characterised in that: the acetic acid replaces with salt
Acid or nitric acid；The dosage of the hydrochloric acid or nitric acid is the 1/6-1/8 of acetic acid volume.
3. SnO according to claim 12The preparation method of nano-powder, it is characterised in that: it is described be slowly added dropwise for by
Drop is added dropwise.
4. SnO according to claim 12The preparation method of nano-powder, it is characterised in that: the revolving speed of the stirring is
100-600r/min。
5. the SnO of the preparation of method described in any one of claim 1-42Nano-powder.
6. SnO according to claim 52Nano-powder, it is characterised in that: the SnO2The average grain diameter of nano-powder
For 3.42nm-22.42nm.
7. a kind of transparent gas sensor, it is characterised in that: utilize SnO described in claim 5 or 62Nano-powder preparation.
8. the preparation method of transparent gas sensor as claimed in claim 7, characterized by the following steps:
(1) by SnO prepared in claim 5 or 62Nano-powder is mixed with water, is added coalescing agent, is prepared into slurry；
(2) slurry that step (1) obtains is coated uniformly on glass carrier, after dry, obtains SnO2Nano coating；
(3) SnO obtained in step (2)2The surface of nano coating applies Ag electrode, is prepared into transparent gas sensor；
Wherein, SnO2Nano-powder: water: the mass ratio of coalescing agent is 1:1-2:0.05-0.2；SnO2The area and slurry of coating
Proportionate relationship be 5-20cm2: 1g.
9. the preparation method of transparent gas sensor according to claim 8, it is characterised in that: dry temperature is 250
DEG C, the dry time is 1-3h.
10. the preparation method of transparent gas sensor according to claim 8, it is characterised in that: the coalescing agent is
Ester alcohol 12；The glass carrier is silica glass carrier.
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