CN105985637A - Manufacturing method of high-sensitivity stable gas sensitive sensor material - Google Patents
Manufacturing method of high-sensitivity stable gas sensitive sensor material Download PDFInfo
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- CN105985637A CN105985637A CN201510065916.XA CN201510065916A CN105985637A CN 105985637 A CN105985637 A CN 105985637A CN 201510065916 A CN201510065916 A CN 201510065916A CN 105985637 A CN105985637 A CN 105985637A
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Abstract
The invention discloses a manufacturing method of a high-sensitivity stable gas sensitive sensor material. The manufacturing method comprises 1, raw material pretreatment, 2, drying for alpha-phase ferric oxide preparation, 3, polypyrrole hybrid material preparation and 4, gas-sensitive sensor material preparation. The alpha-phase ferric oxide prepared through a dissolution-recrystallization mechanism has the advantages of high particle purity, good dispersibility and good crystal form. The manufacturing method has simple processes and mild and easily controlled conditions, realizes a low cost, is free of a surfactant and reduces impurity ion-caused influence on products. The tin oxide-polypyrrole hybrid material product can be purified easily and has good gas-sensitive selectivity at a low work temperature, and through combination of the alpha-phase ferric oxide and the hybrid material, the hybrid material and saturated pyrrole steam undergo a reaction so that the surface of the tin dioxide-polypyrrole hybrid material is covered with a PPy sensitive material and thus gas sensor sensitivity and stability to gas such as NH3 and NO2 are effectively improved.
Description
Technical field
The invention belongs to sensor material preparing technical field, be specifically related to the manufacture method of a kind of high sensitivity stable type gas sensor material.
Background technology
Gas sensor is a kind of transducer that certain gas volume fraction changes into the corresponding signal of telecommunication.Gaseous sample is nursed one's health by detecting head by gas sensor, generally includes and filters impurity and interference gas, is dried or refrigeration processes instrument display part and divides.Gas sensor is a kind of device that the information such as the composition of gas, concentration are converted into the information that can be utilized by personnel, instrument and meter, computer etc.." gas sensor " including: semiconductor gas sensor, electrochemical gas sensor, catalytic combustion method gas sensor, thermal conductivity gas sensor, infrared gas sensor etc..
Now the oxide for acetone vapor sensitive material mainly has ZnO, SnO2、Ga2O3、CeO2, NiO etc., made acetone gas sensor also exists the defect that operating temperature is higher, power consumption is bigger mostly.Such as, WO3-ZnO and MoO3The operating temperature of-ZnO is 500 DEG C, CdIn2O4
Operating temperature be 350 DEG C, Eu2O3-
SnO2Operating temperature is 185 DEG C.In prior art, it is used for detecting NH3And NO2Conductor oxidate is mainly included, such as ZnO, SnO Deng the sensitive materials of gas2, NiO etc. and their alloy, but they mostly can not work at normal temperatures, it usually needs and it is heated to specific temperature, improves power consumption；Organic polymer, as PPy, Polyaniline (PANI) may also be used for detecting NH3And NO2, and it the most just can work, but organic polymer film forming is more difficult, and stability is not so good as conductor oxidate sensitive material.Alpha-phase ferricoxide, is commonly called as bloodstone, is the most most stable of ferrum oxide.The performance such as anticorrosive of nontoxic, the environmental friendliness that has due to himself and excellence and receive much concern, thus also it is provided with wide application prospect, the field such as relevant with magnetic recording material in coating, gas sensor material, lithium ion battery negative material, catalyst.
Summary of the invention
For the problems of the prior art, the purpose of the present invention aims to provide the manufacture method of a kind of high sensitivity stable type gas sensor material, the alpha-phase ferricoxide of preparation has the advantages such as particle purity height, good dispersion and crystal formation are good, tin ash polypyrrole hybrid material and the combination of alpha-phase ferricoxide, saturated vapor pyrroles reacts and makes its surface be coated with the sensitive material of PPy, is effectively improved gas sensor to NH3And NO2Sensitivity and stability Deng gas.
The technical scheme that the present invention takes is:
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: in a kettle., the ferric nitrate that concentration is 30mmol/L-50mmol/L and the glucose that concentration is 45mmol/L-90mmol/L mixing is taken according to volume ratio 2:1, add appropriate amount of deionized water, be configured to the mixed solution of 80mmol/L, stir；
(2) dry alpha-phase ferricoxide processed: be placed in by reactor in 160-180 ° of C baking oven, insulation reaction 1.3-1.5h, be cooled to room temperature, then take out and product respectively washed 3 times with distilled water and dehydrated alcohol respectively, dry in 60 DEG C of baking ovens；
(3) polypyrrole hybrid material processed: take tin ash and pyrrole monomer mixed grinding according to weight ratio 2:5, with deionized water furnishing pasty state, immerses containing 30% FeCl3Ethanol solution in react 2-2.5h, standby；
(4) gas sensor material processed: take polypyrrole hybrid material and alpha-phase ferricoxide mixing according to weight ratio 1:3, add the hydrochloric acid solution of 3 times of volume 0.4mol/L-0.6mol/L, after ultrasonic 30min-50min, proceed to reactor, reactor is placed in 150 DEG C of-170 DEG C of baking ovens, hydro-thermal reaction 7-8h, puts into 4-6h in the saturated vapor of pyrroles.
Further, in described step (3) tin ash and pyrrole monomer mixed grinding to less than 80nm-120nm.
Further, FeCl in described step (3)3Concentration be 0.06-0.08mol/L.
The invention have the benefit that
The alpha-phase ferricoxide that the present invention utilizes the mechanism of dissolution-recrystallization to prepare has the advantages such as particle purity height, good dispersion and crystal formation are good, processing technology is simple, and mild condition is easily-controllable, with low cost, there is no the participation of surfactant, reduce the foreign ion impact on product.
Tin ash can get the tin ash polypyrrole hybrid material of different polypyrrole mass fraction from pyrrole monomer hybrid reaction, product is prone to purification, at lower operating temperatures gas can be had good air-sensitive selectivity, its combination with alpha-phase ferricoxide, saturated vapor pyrroles reacts and makes its surface be coated with the sensitive material of PPy, is effectively improved gas sensor to NH3 And NO2 Sensitivity and stability Deng gas.
Detailed description of the invention
Embodiment 1
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: in a kettle., takes the ferric nitrate that concentration is 30mmol/L and the glucose that concentration is 45mmol/L mixing according to volume ratio 2:1, adds appropriate amount of deionized water, be configured to the mixed solution of 80mmol/L, stir；
(2) dry alpha-phase ferricoxide processed: be placed in by reactor in 160 ° of C baking ovens, insulation reaction 1.5h, be cooled to room temperature, then take out and product respectively washed 3 times with distilled water and dehydrated alcohol respectively, dry in 60 DEG C of baking ovens；
(3) polypyrrole hybrid material processed: take tin ash and pyrrole monomer mixed grinding according to weight ratio 2:5, with deionized water furnishing pasty state, immersing containing 30% concentration is the FeCl of 0.06mol/L3Ethanol solution in react 2h, standby；
(4) gas sensor material processed: take polypyrrole hybrid material and alpha-phase ferricoxide mixing according to weight ratio 1:3, add the hydrochloric acid solution of 3 times of volume 0.4mol/L, after ultrasonic 30min, proceed to reactor, reactor is placed in 150 DEG C of baking ovens, hydro-thermal reaction 8h, puts into 4h in the saturated vapor of pyrroles.
Further, in described step (3) tin ash and pyrrole monomer mixed grinding to less than 80nm-120nm.
Embodiment 2
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: in a kettle., takes the ferric nitrate that concentration is 40mmol/L and the glucose that concentration is 70mmol/L mixing according to volume ratio 2:1, adds appropriate amount of deionized water, be configured to the mixed solution of 80mmol/L, stir；
(2) dry alpha-phase ferricoxide processed: be placed in by reactor in 170 ° of C baking ovens, insulation reaction 1.4h, be cooled to room temperature, then take out and product respectively washed 3 times with distilled water and dehydrated alcohol respectively, dry in 60 DEG C of baking ovens；
(3) polypyrrole hybrid material processed: take tin ash and pyrrole monomer mixed grinding according to weight ratio 2:5, with deionized water furnishing pasty state, immersing containing 30% concentration is the FeCl of 0.07mol/L3Ethanol solution in react 2.3h, standby；
(4) gas sensor material processed: take polypyrrole hybrid material and alpha-phase ferricoxide mixing according to weight ratio 1:3, add the hydrochloric acid solution of 3 times of volume 0.5mol/L, after ultrasonic 40min, proceed to reactor, reactor is placed in 160 DEG C of baking ovens, hydro-thermal reaction 7.5h, puts into 5h in the saturated vapor of pyrroles.
Further, in described step (3) tin ash and pyrrole monomer mixed grinding to less than 80nm-120nm.
Embodiment 3
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: in a kettle., takes the ferric nitrate that concentration is 50mmol/L and the glucose that concentration is 90mmol/L mixing according to volume ratio 2:1, adds appropriate amount of deionized water, be configured to the mixed solution of 80mmol/L, stir；
(2) dry alpha-phase ferricoxide processed: be placed in by reactor in 180 ° of C baking ovens, insulation reaction 1.3h, be cooled to room temperature, then take out and product respectively washed 3 times with distilled water and dehydrated alcohol respectively, dry in 60 DEG C of baking ovens；
(3) polypyrrole hybrid material processed: take tin ash and pyrrole monomer mixed grinding according to weight ratio 2:5, with deionized water furnishing pasty state, immersing containing 30% concentration is the FeCl of 0.08mol/L3 Ethanol solution in react 2.5h, standby；
(4) gas sensor material processed: take polypyrrole hybrid material and alpha-phase ferricoxide mixing according to weight ratio 1:3, add the hydrochloric acid solution of 3 times of volume 0.6mol/L, after ultrasonic 50min, proceed to reactor, reactor is placed in 170 DEG C of baking ovens, hydro-thermal reaction 7h, puts into 6h in the saturated vapor of pyrroles.
Further, in described step (3) tin ash and pyrrole monomer mixed grinding to less than 80nm-120nm.
Claims (3)
1. the manufacture method of a high sensitivity stable type gas sensor material, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: in a kettle., the ferric nitrate that concentration is 30mmol/L-50mmol/L and the glucose that concentration is 45mmol/L-90mmol/L mixing is taken according to volume ratio 2:1, add appropriate amount of deionized water, be configured to the mixed solution of 80mmol/L, stir；
(2) dry alpha-phase ferricoxide processed: be placed in by reactor in 160-180 ° of C baking oven, insulation reaction 1.3-1.5h, be cooled to room temperature, then take out and product respectively washed 3 times with distilled water and dehydrated alcohol respectively, dry in 60 DEG C of baking ovens；
(3) polypyrrole hybrid material processed: take tin ash and pyrrole monomer mixed grinding according to weight ratio 2:5, with deionized water furnishing pasty state, immerses containing 30% FeCl3Ethanol solution in react 2-2.5h, standby；
(4) gas sensor material processed: take polypyrrole hybrid material and alpha-phase ferricoxide mixing according to weight ratio 1:3, add the hydrochloric acid solution of 3 times of volume 0.4mol/L-0.6mol/L, after ultrasonic 30min-50min, proceed to reactor, reactor is placed in 150 DEG C of-170 DEG C of baking ovens, hydro-thermal reaction 7-8h, puts into 4-6h in the saturated vapor of pyrroles.
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that in described step (3), tin ash and pyrrole monomer mixed grinding are to less than 80nm-120nm.
The manufacture method of a kind of high sensitivity stable type gas sensor material, it is characterised in that FeCl in described step (3)3Concentration be 0.06-0.08mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880318A (en) * | 2017-11-07 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and products thereof and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880318A (en) * | 2017-11-07 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of hydrogen sulfide gas sensing material of biomass carrying inorganic particle and products thereof and application |
| CN107880318B (en) * | 2017-11-07 | 2020-02-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of biomass loaded inorganic particle hydrogen sulfide gas sensing material, product and application thereof |
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