CN109115834A - A kind of ppb grades of NO2Gas sheet type sensor and preparation method - Google Patents
A kind of ppb grades of NO2Gas sheet type sensor and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of ppb grades of NO2Gas sheet type sensor and preparation method pass through the synthesising mesoporous WO of hard template method3;Using YSZ as solid electrolyte, mesoporous WO3NO is made for sensitive electrode2Gas sheet type sensor.NO prepared by the present invention2Sheet type sensor has many advantages, such as simple structure, high sensitivity, detects limit low (60ppb), is selective and reproducible.
Description
Technical field
The present invention relates to NO2Sensor technical field, especially a kind of mesoporous tungsten oxide is as sensitive electrode NO2Gas piece
The preparation method of formula sensor.Mesoporous WO3Powder is made by hard template method, then with mesoporous WO3NO is prepared for sensitive electrode2Piece
Formula sensor.
Background technique
With the development of economy and society, environmental pollution is increasingly severe.The combustion-type NO of fossil fuel2Pollutant it is main
Source.NO2It would generally cause acid rain and photochemical fog, seriously threaten the ecological balance and the health of the mankind.Many countries
Environmental legislation mention, NO in air2Maximum acceptable concentration be 5ppm.NO in atmosphere2Concentration be about 0.01ppm, but U.S.
Environmental Protection Department think be more than 0.65ppm NO2There is sizable threat to human health.Environmental Protection Agency is also shown that
Child on long-term, which is exposed to 53ppb or more, will lead to serious breathing problem.Therefore, China more payes attention to environmental improvement, urgent uncommon
It hopes and develops highly sensitive, ppb grades NO2Sensor.NO at present2Detection method have infra-red sepectrometry, chemoluminescence method etc., this
A little method instruments are complicated, are not easy on-line continuous monitoring.In comparison electrochemistry sheet type sensor is because its structure is simple, cost
It is low, can on-line continuous monitoring and have been to be concerned by more and more people.Sound of the sensitive electrode to sensor in electrochemical sensor
Answer, sensitivity and selectivity etc. all have a great impact.But general electrochemical sensor can only detect ppm grades of NO2, can not
Fully meet the requirement of environment measuring (ppb grades).
Summary of the invention
The object of the present invention is to provide a kind of ppb grades of (60ppb) NO of high sensitivity2Gas sheet type sensor and preparation side
Method, preparation method is with mesoporous WO3NO is made for sensitive electrode2Gas sheet type sensor;Its NO2Sheet type sensor has structure
Simply, be readily synthesized, high sensitivity, detection limit it is low, selectivity and it is reproducible the advantages that.
Realizing the specific technical solution of the object of the invention is:
A kind of ppb grades of NO of high sensitivity2The preparation method of gas sheet type sensor, this method comprising the following specific steps
Step 1: the preparation of hard template SBA-15
ⅰ)P123(EO20PO70EO20) and 2mol/L HCl, H2O is mixed according to mass ratio 2:60:15, stirs 30-60min
It is completely dissolved to P123;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, according to solution and ethyl orthosilicate
(TEOS) ethyl orthosilicate, 40 DEG C of stirring 24-48h are added dropwise in mass ratio 20:1;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reaction 12-24h are filtered, washed, 80 DEG C of dry 12-24h;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 6-10h obtain SBA-15;
Step 2: mesoporous WO3Synthesis
I) silico-tungstic acid with ethyl alcohol is that 7:20 is mixed in mass ratio, stirring to silico-tungstic acid is dissolved;
II) SBA-15 adds to I) obtained in silico-tungstic acid solution (mass ratio 1:5), ultrasonic 10-30min, by SBA-
Bubble discharge in 15 ducts;
III) II) obtained in solution stir 12-24h at room temperature, dry 12-24h at 80 DEG C, then 550 DEG C of burning 4h, obtain
To solid mixture;
IV) HF and H2O is mixed to get the HF solution of 3mol/L according to volume ratio 1:11.III) obtained in solid and 3mol/
The HF solution of L is mixed according to mass ratio 1:30, stirs 12-24h, and filtration washing naturally dry obtains mesoporous WO3;
Step 3:NO2The preparation of gas sheet type sensor
I) mesoporous WO3It is mixed with ethyl cellulose and terpinol according to mass ratio 10:1:20, with planet vibrator
100r/min ball milling 2-5h, obtains mesoporous WO3Slurry.
II) 8YSZ (8%Y2O3Adulterate ZrO2) cast sheet is cut into the thin slice of 1 × 1cm, tow sides are stamped with silk-screen printing
Pt electrode, and Pt are drawn respectively from two electrodes, 1400 DEG C of burning 2-4h in Muffle furnace;
III) by II) obtained in the side of piece pass through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and in Muffle
2-4h is burnt in furnace at 600 DEG C and obtains ppb grades of NO2Gas sheet type sensor.
With mesoporous WO3Do sensitive electrode, the sensitivity of sheet type sensor greatly improves that (S=51.76mV/decade, S are
The slope of working curve, working curve are△ EMF is sensor in NO2In
It is NO with the potential difference C in background gas2The concentration b of gas is the intercept of working curve), favorable reproducibility, stability height.
The present invention is using SBA-15 as the mesoporous WO of templated synthesis3Sensitive electrode, and NO is assembled with it2Sheet type sensor;It reduces
The detectable limit (ppb grades) of sensor, improves the sensitivity of sensor.Sheet type sensor structure produced by the present invention is simple,
It is at low cost, the production efficiency of sensor can be greatly improved, convenient for integrated.
Detailed description of the invention
Fig. 1 is mesoporous WO prepared by the embodiment of the present invention 43XRD diagram;
Fig. 2 is mesoporous WO prepared by the embodiment of the present invention 43TEM figure;
Fig. 3 is the working curve of sensor prepared by inventive embodiments 4;
Fig. 4 is sensor made from the embodiment of the present invention 4, and test temperature is the reperformance test knot in 30 days at 500 DEG C
Fruit figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
(a) preparation of hard template SBA-15
ⅰ)4g P123(EO20PO70EO20) it is dissolved in the HCl+30g H that 120g concentration is 2mol/L2In the solution of O, stirring
30min to P123 is completely dissolved;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, 7.52g ethyl orthosilicate is added dropwise
(TEOS), it stirs for 24 hours for 40 DEG C;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reaction 12h are filtered, washed, 80 DEG C of dry 12h;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 6h obtain SBA-15;
(b) mesoporous WO3Synthesis
I) 1.75g silico-tungstic acid is dissolved in 5g ethyl alcohol;
II) 1g SBA-15 adds to 5g I) obtained in silico-tungstic acid solution, ultrasonic 10min, by the gas in the duct SBA-15
Bubble discharge;
III) by II) obtained in solution stir 12h, dry 12h at 80 DEG C at room temperature, then 550 DEG C of burning 4h, consolidate
Body mixture;
IV) by 1g III) obtained in solid 12h filtration washing naturally dry is stirred in the solution of 30gHF, obtain mesoporous
WO3;
(c)NO2The preparation of gas sheet type sensor
I) the mesoporous WO of 0.5g3It is mixed with 0.05g ethyl cellulose and 1g terpinol, with planet vibrator 100r/min
Ball milling 2h obtains mesoporous WO3Slurry;
II) 8YSZ (8%Y2O3Adulterate ZrO2) cast sheet is cut into the thin slice of 1 × 1cm, tow sides are stamped with silk-screen printing
Pt electrode, and Pt are drawn respectively from two electrodes, 1400 DEG C of burning 2h in Muffle furnace;
III) II) obtained in the side of piece pass through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and in Muffle furnace
In burn 2h at 600 DEG C and obtain NO2Sheet type sensor;
(d) gained NO2Sheet type sensor is when operating temperature is 500 DEG C, to 0.06-10ppmNO2Sensitivity reach
47mV/decade。
Embodiment 2
(a) preparation of hard template SBA-15
ⅰ)32g P123(EO20PO70EO20) it is dissolved in the HCl+240g H that 960g concentration is 2mol/L2In the solution of O, stir
60min to P123 is mixed to be completely dissolved;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, 60.16g ethyl orthosilicate is added dropwise
(TEOS), 40 DEG C of stirring 48h;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reactions for 24 hours, are filtered, washed, 80 DEG C of dryings are for 24 hours;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 10h obtain SBA-15;
(b) mesoporous WO3Synthesis
I) 14g silico-tungstic acid is dissolved in 40g ethyl alcohol;
II) 8g SBA-15 adds to 40g I) obtained in silico-tungstic acid solution, ultrasonic 30min will be in the duct SBA-15
Bubble discharge;
III) by II) obtained in solution stir at room temperature for 24 hours, at 80 DEG C it is dry for 24 hours, then 550 DEG C of burning 4h, consolidate
Body mixture;IV) by 8g III) obtained in solid stirred for 24 hours in 240gHF solution, filtration washing naturally dry is situated between
Hole WO3;
(c)NO2The preparation of gas sheet type sensor
I) the mesoporous WO of 4g3It is mixed with 0.4g ethyl cellulose and 8g terpinol, with planet vibrator 100r/min ball
5h is ground, mesoporous WO is obtained3Slurry;
II) 8YSZ (8%Y2O3Adulterate ZrO2) cast sheet is cut into the thin slice of 1 × 1cm, tow sides are stamped with silk-screen printing
Pt electrode, and Pt are drawn respectively from two electrodes, 1400 DEG C of burning 4h in Muffle furnace;
III) by II) obtained in the side of piece pass through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and in Muffle
4h is burnt in furnace at 600 DEG C and obtains NO2Sheet type sensor;
(d) gained NO2Sheet type sensor is when operating temperature is 500 DEG C, to 0.06-10ppmNO2Sensitivity reach
48.2mV/decade。
Embodiment 3
(a) preparation of hard template SBA-15
ⅰ)16g P123(EO20PO70EO20) it is dissolved in the HCl+120g H that 480g concentration is 2mol/L2In the solution of O, stir
50min to P123 is mixed to be completely dissolved;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, 30.08g ethyl orthosilicate is added dropwise
(TEOS), 40 DEG C of stirring 40h;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reaction 20h are filtered, washed, 80 DEG C of dry 20h;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 9h obtain SBA-15;
(b) mesoporous WO3Synthesis
I) 7g silico-tungstic acid is dissolved in 20g ethyl alcohol;
II) 4g SBA-15 adds to 20g I) obtained in silico-tungstic acid solution, ultrasonic 25min will be in the duct SBA-15
Bubble discharge;
III) by II) obtained in solution stir 20h, dry 20h at 80 DEG C at room temperature, then 550 DEG C of burning 4h, consolidate
Body mixture;
IV) by 4g III) obtained in solid 20h is stirred in the solution of 120gHF, filtration washing naturally dry is situated between
Hole WO3;
(c)NO2The preparation of gas sheet type sensor
I) by the mesoporous WO of 2g3It is mixed with 0.2g ethyl cellulose and 4g terpinol, with planet vibrator 100r/min
Ball milling 4h obtains mesoporous WO3Slurry;
II) 8YSZ (8%Y2O3Adulterate ZrO2) cast sheet is cut into the thin slice of 1 × 1cm, tow sides are stamped with silk-screen printing
Pt electrode, and Pt are drawn respectively from two electrodes, 1400 DEG C of burning 3.5h in Muffle furnace;
III) by II) obtained in the side of piece pass through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and in Muffle
3.5h is burnt in furnace at 600 DEG C and obtains NO2Sheet type sensor;
(d) gained NO2Sheet type sensor is when operating temperature is 500 DEG C, to 0.06-10ppmNO2Sensitivity reach
49mV/decade。
Embodiment 4
(a) preparation of hard template SBA-15
ⅰ)8g P123(EO20PO70EO20) it is dissolved in the HCl+60g H that 240g concentration is 2mol/L2In the solution of O, stirring
40min to P123 is completely dissolved;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, 15.04g ethyl orthosilicate is added dropwise
(TEOS), 40 DEG C of stirring 36h;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reaction 16h are filtered, washed, 80 DEG C of dry 16h;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 8h obtain SBA-15;
(b) mesoporous WO3Synthesis
I) 3.5g silico-tungstic acid is dissolved in 10g ethyl alcohol;
II) 2g SBA-15 adds to 10g I) obtained in silico-tungstic acid solution, ultrasonic 20min will be in the duct SBA-15
Bubble discharge;
III) by II) obtained in solution stir 16h, dry 16h at 80 DEG C at room temperature, then 550 DEG C of burning 4h, consolidate
Body mixture;
IV) by 2g III) obtained in solid 16h is stirred in the solution of 60ml 3mol/LHF, filtration washing dries in the air naturally
It is dry, obtain mesoporous WO3;It can be seen that the mesoporous WO that the present invention synthesizes by the XRD in Fig. 13For monocline WO3, cell parameter is andDo not occur SiO in XRD2Peak, pattern of descriptive parts removes more thorough
Bottom.The mesoporous WO of Fig. 23TEM can be seen that mesoporous WO3There is elongated pipeline, aperture is 7nm or so.
(c)NO2The preparation of gas sheet type sensor
I) by the mesoporous WO of 1g3It is mixed with 0.1g ethyl cellulose and 2g terpinol, with planet vibrator 100r/min
Ball milling 3h obtains mesoporous WO3Slurry;
II) 8YSZ (8%Y2O3Adulterate ZrO2) cast sheet is cut into the thin slice of 1 × 1cm, tow sides are stamped with silk-screen printing
Pt electrode, and Pt are drawn respectively from two electrodes, 1400 DEG C of burning 2h in Muffle furnace;
III) by II) obtained in the side of piece pass through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and in Muffle
2h is burnt in furnace at 600 DEG C and obtains NO2Sheet type sensor;
(d) from figure 3, it can be seen that testing at 500 DEG C sensor, to 0.06-10ppmNO2Sensitivity reach
51.76mV/decade, degree of fitting reach 99.4%.From fig. 4, it can be seen that be repeated four times test in 30 days, working curve it is oblique
Rate is basically unchanged (between 50.94-51.76), and intercept changes very small (between 72.7-75.1), and four times test curve weighs substantially
It is combined.Illustrate that sensor has repeatability and stability well.
Claims (2)
1. a kind of ppb grades of NO2The preparation method of gas sheet type sensor, which is characterized in that this method comprising the following specific steps
Step 1: the preparation of hard template SBA-15
I) EO20PO70EO20That is HCl, H of P123 and 2mol/L2O is mixed according to mass ratio 2:60:15, and stirring 30-60min is extremely
P123 is completely dissolved;
II) by I) in solution be put into water-bath, when temperature reaches 40 DEG C, according to solution and ethyl orthosilicate (TEOS) matter
Ethyl orthosilicate, 40 DEG C of stirring 24-48h are added dropwise than 20:1 in amount;
III) by II) in solution be transferred to reaction kettle, 100 DEG C of reaction 12-24h are filtered, washed, 80 DEG C of dry 12-24h;
IV) dried powder is placed in Muffle furnace, 550 DEG C of burning 6-10h obtain SBA-15;
Step 2: the synthesis of mesoporous tungsten oxide
I) silico-tungstic acid with ethyl alcohol is that 7:20 is mixed in mass ratio, stirring to silico-tungstic acid is dissolved;
II) SBA-15 added into I) obtained in silico-tungstic acid solution, ultrasonic 10-30min arranges the bubble in the duct SBA-15
Out;The SBA-15 and silico-tungstic acid mass ratio are 1:5;
III) by II) obtained in solution stir 12-24h at room temperature, dry 12-24h at 80 DEG C, then 550 DEG C of burning 4h, obtain
Solid mixture;
IV) HF and H2O is mixed to get the HF solution of 3mol/L according to volume ratio 1:11;By III) obtained in solid and 3mol/L
HF solution mixed according to mass ratio 1:30, stir 12-24h, filtration washing naturally dry obtains mesoporous WO3;
Step 3: preparation NO2Gas sheet type sensor
I) by mesoporous WO3It mixes with ethyl cellulose and terpinol, with planet vibrator 100r/min ball milling 2-5h, obtains
Mesoporous WO3Slurry;The mesoporous WO3, ethyl cellulose and terpinol mass ratio 10:1:20;
II) 8YSZ cast sheet is cut into the thin slice of 1 × 1cm, tow sides stamp Pt electrode with silk-screen printing, and from two electrodes
Place draws Pt respectively, 1400 DEG C of burning 2-4h in Muffle furnace;The 8YSZ is 8%Y2O3Adulterate ZrO2;
III) by II) one side of gained thin slice passes through mesoporous WO in silk-screen printing on platinum slurry3Slurry, and 600 DEG C in Muffle furnace
Lower burning 2-4h obtains the ppb grades of NO2Gas sheet type sensor.
2. ppb grades of NO made from a kind of claim 1 the method2Gas sheet type sensor.
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CN111044582A (en) * | 2019-12-04 | 2020-04-21 | 中国工程物理研究院化工材料研究所 | Fluorocarbon film/metal oxide gas-sensitive film composite laminated device and preparation method thereof |
CN114994152A (en) * | 2022-05-18 | 2022-09-02 | 上海应用技术大学 | Preparation method of high-sensitivity electrochemical nitrogen dioxide gas sensor with mesoporous tungsten oxide as sensitive electrode |
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