CN107817277A - The preparation method of new high selectivity acetone gas sensor - Google Patents

The preparation method of new high selectivity acetone gas sensor Download PDF

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Publication number
CN107817277A
CN107817277A CN201610819844.8A CN201610819844A CN107817277A CN 107817277 A CN107817277 A CN 107817277A CN 201610819844 A CN201610819844 A CN 201610819844A CN 107817277 A CN107817277 A CN 107817277A
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gas sensor
colloid
preparation
solution
coo
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潘国峰
李菲
陈静
李洋洋
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Hebei University of Technology
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Hebei University of Technology
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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

Abstract

The present invention relates to a kind of preparation method of new high selectivity acetone gas sensor, there is field prepared by the gas sensing device of high selection characteristic suitable for acetone steam.The present invention uses sol-gal process, is preparing doping Zn (OH)2During colloid, cetyl trimethylammonium bromide is added, then dries and grinds by colloid, cleaning, high annealing, obtained material gas sensor is made, carries out aging with cetyl trimethylammonium bromide coated on earthenware after process annealing.Adding cetyl trimethylammonium bromide in colloid preparation process helps to generate stable colloid；Coated in cetyl trimethylammonium bromide is used on earthenware, adhesive effect is played, and the sensitivity of gas sensor can be being improved by process annealing, cetyl trimethylammonium bromide.Gas sensor prepared by the present invention has sensitivity characteristic to acetone vapor, can detect acetone vapor in numerous organic vapors.

Description

The preparation method of new high selectivity acetone gas sensor
Technical field：
There is the preparation method of the gas sensing device of high selection characteristic the invention belongs to a kind of acetone steam.
Technical background：
As social environment consciousness is progressively strengthened, gas sensor has been widely used in the oil, chemical industry, smelting of the country The industries such as gold, pharmacy, food, medical treatment, road traffic, municipal combustion gas, digital mine.Oxide semiconductor gas sensor, by In its high sensitivity, the features such as fast, small volume, energy consumption and cost are low, simple to operate is responded, is widely used in various target gas In the detection of body.The preparation technology of material is very big on air-sensitive performance influence, and corresponding form has slug type, thick-film type and film Type.The nano material that at present prepared by laboratory includes nano particle, nano wire, nanobelt, nano-rings, nanotube, nanochannel With hole etc..Acetone is a kind of industry and the widely used organic solvent in laboratory, has height inflammability, Long Term Contact can be right Human body causes significant damage.At present, there is poor selectivity in the domestic acetone sensor developed, and homogeneity of product is poor, and sensitivity is low, The response-recovery time is grown, and effective industrialization is not formed also for the dedicated sensor of acetone gas.Domestic preparation method Mostly sputtering method, preparation method of the present invention prepare gas sensor element, and method is convenient, and cost is cheap, stable performance, It is suitable for industrial production.
Gas sensor prepared by the present invention has high selectivity to acetone vapor, good to the sensitivity characteristic of acetone, and right It is substantially insensitive that machine steam (such as ethanol, ammonia, formaldehyde etc.) is common are in other, it is possible to achieve can be organic in numerous mixing In steam, presence or absence and its concentration of acetone vapor are detected.
The content of the invention：
This gas sensitive device prepares aluminium doping Zn (OH) using sol-gel process2Colloid, the chemical reaction of colloid preparation process Principle is：
Zn2++2OH-→Zn(OH)2
Al3++3OH-→Al(OH)3
Zn(CH3COO)·2H2O→Zn(C2H3O2)-→Zn(OH)2→ZnO
Al(NO3)3·9H2O→Al3+→Al(OH)3→Al2O3
The present invention preparation method be：
A. doping Zn (OH) is prepared2Colloid：Absolute ethyl alcohol is mixed with deionized water according to 1: 1-1: 2 volume ratio, As solvent；With Zn (CH3COO)2·2H2O crystal is as solute, configuration Zn (CH3COO)2Solution, concentration range 0.8- 1mol/L；
By cetyl trimethylammonium bromide and Zn (CH3COO)2Solution is mixed with 1: 4-1: 5 volume ratio
With Al (NO3)3·9H2O is 4-5wt% as dopant, doping mass ratio, is added to Zn (CH3COO)2In solution Mixing；
With mixer agitating solution, rotating speed instills NaOH solution with 0.1-1ml/min drop speed, used in 80-150r/min In adjusting pH value, stop instilling as pH=7, continue to stir 0.5-1 hours, close agitator, stand 24 hours and obtain colloid.Institute NaOH solution and Zn (CH3COO)2Solution mol ratio is 2: 1, and solvent for use is similarly absolute ethyl alcohol with deionized water according to 1 : the solvent of 1-1: 2 volume ratio mixing.
B. it is solid with oven for drying by colloid, temperature is 80-100 DEG C, hour time 2-3, then by solid abrasive 15- 20min is into powder；Powder is cleaned with deionized water, and filtered with filter paper, 300 DEG C of process annealing 1-2 are small in horse takes stove When, powder 15-20 minutes are regrind, cleaning process is in triplicate；Powder after cleaning is put into horse expense stove and carries out 600- 800 DEG C of high annealing 2-3 hours, Al is made2O3The ZnO powder material of doping.
C. material is mixed at 4: 1-5: 1 by volume with cetyl trimethylammonium bromide, is then coated with having welded in wire The centre (3) for the earthenware (1) being connected on pedestal, coating thickness 1-100um；Earthenware is put into horse expense stove and carried out 250-300 DEG C of process annealing 10-30 minutes, obtain Al2O3The zno-based high selectivity acetone gas sensor of doping.Used Earthenware is tested for gas-sensitive property, and earthenware (1) is built-in with heater strip (4), is welded in the heating circuit of pedestal, heater strip (4) it is used for improving the operating temperature of sensor, the platinum wire wire (2) at earthenware both ends is welded in the pressurization circuit of pedestal, For detecting the change of earthenware resistance.Utilize Al2O3When-ZnO gas sensors surface is with absorption acetone steam, resistance can be with it Change in concentration and the principle changed, detect the content of acetone among environment.
D. obtained gas sensor is subjected to temperature and humidity control aging, temperature is 75-99 DEG C, relative humidity 30%-70% RH, 5-7 days time.
The present invention has the following advantages compared with prior art：
(1) present invention is preparing Zn (OH)2Cetyl trimethylammonium bromide is added during colloid, contribute into Stable colloid is formed in glue, and during colloid is dried into solid, the knot of the cetyl trimethylammonium bromide added Structure can limit growing up for crystal grain, be easily formed nanocrystal.
(2) present invention uses cetyl trimethylammonium bromide when by material coated on earthenware, not only acts as viscous The effect of mixture, and after process annealing, outside a part of cetyl trimethylammonium bromide oxidation discharge film, increase Meso-hole structure, improve the specific surface area of material；Meanwhile a part of C enters lattice as dopant, it is composite mixed to form Al, C ZnO, so as to improve the sensitivity of gas sensor.
(3) present invention improves the stability of sensor by carrying out senile experiment to gas sensor.
(4) preparation method is simple, and cost is low.The present invention prepares colloid using sol-gel process, and room temperature can meet colloid Preparation condition, and there is very high selectivity, sensitivity and stability to acetone.
Main application：Detect acetone steam and its concentration.
Brief description of the drawings：
Fig. 1 is the earthenware structure chart of high selectivity acetone gas sensor
1. earthenware in figure, 2. earthenware both ends platinum wire wires, 3.ZnO materials, 4. heater strips.
Embodiment：
Embodiment 1：
1. prepare colloid
(1) configuration prepares the solvent of colloid.Absolute ethyl alcohol is mixed with deionized water according to 1: 1 volume ratio, stirred To uniform.
(2) Zn (CH are weighed respectively with electronic balance3COO)2·2H2O crystal and NaOH crystal, and respectively with preparing Solvent mixes, and obtained concentration is respectively 0.8mol/L and 1.6mol/L solution.
(3) w (Al are weighed with electronic balance2O3) be 4.5wt% Al (NO3)3·9H2O is mixed into Zn (CH3COO)2Solution In；
(4) by cetyl trimethylammonium bromide and Zn (CH3COO)2Solution is mixed with 1: 5 ratio；
(5) Zn (CH are stirred with mixer3COO)2Solution, rotating speed about 100r/min, by NaOH solution with 0.1ml/min's Drop speed instills Zn (CH3COO)2Solution, stop when detecting solution to pH=7 with pH test paper；
(6) continue stirring 0.5 hour after forming colloid, close agitator, stand colloid and obtain colloid after 24 hours.
2. drying grinding colloid
(1) it is 100 DEG C by colloid oven for drying, temperature, time 2 h, is dried into solid.It should be noted that it is Prevent colloid from splashing, initial temperature because less than 50 DEG C, being transferred to 100 DEG C again after the moisture evaporation in colloid；
(2) by solid abrasive 15min into powder.
3. cleaning
(1）Powder is poured into deionized water and stirred, is completely dissolved the impurity in powder, is stayed with filter paper sieve more pure Powder residue, wait natural air drying；
(2) by residue 300 DEG C of Muffle furnace process annealing 2 hours, 15min is fully ground in mortar；
(3) cleaning process is repeated 3 times.
4. annealing
Powder is put into Muffle furnace, 700 DEG C of annealing temperature, constant temperature 2 hours, it is required that cooling is taken out after 24 hours Al2O3- ZnO powder body materials.
5. gas sensor is made
(1) earthenware is welded on special pedestal, and by Al2O3- ZnO powder body materials and cetyl trimethyl bromine Change the ratio mixing of ammonium 5: 1, centre (3) place for the earthenware (1) being then applied to, coating thickness 1um；
(2) obtained earthenware being put into process annealing 10min in horse expense stove, annealing temperature is 300 DEG C, constant temperature 10min, Take out to obtain gas sensor after 24 hours；
(3) its gas-sensitive property is determined with HW-30A type air-sensitive testers, during response of the gas sensor of the invention to acetone Between be 1 second, recovery time be 2 seconds.And there is very strong selectivity to acetone, can exclude to measure other in atmosphere common has The interference of machine steam.
6. aging
(1) gas sensor after test is inserted into desk-top gas sensor agingtable, is 4.5V in heating voltage, it is corresponding Heating-up temperature is 75 DEG C, under conditions of relative humidity is 30%RH, aging 7 days.
(2) its gas-sensitive property is determined with HW-30A type air-sensitive testers, gas sensor of the invention has very strong to acetone Selectivity and stability.
Embodiment 2：
1. prepare colloid
(1) configuration prepares the solvent of colloid.Absolute ethyl alcohol is mixed with deionized water according to 1: 2 volume ratio, stirred To uniform.
(2) Zn (CH are weighed respectively with electronic balance3COO)2·2H2O crystal and NaOH crystal, and respectively with preparing Solvent mixes, and obtained concentration is respectively 1mol/L and 2mol/L solution.
(3) w (Al are weighed with electronic balance2O3) be 4wt% Al (NO3)3·9H2O is mixed into Zn (CH3COO)2Solution In；
(4) by cetyl trimethylammonium bromide and Zn (CH3COO)2Solution is mixed with 1: 4 ratio；
(5) Zn (CH are stirred with mixer3COO)2Solution, rotating speed about 80r/min, by NaOH solution with 0.5ml/min drop Speed instills Zn (CH3COO)2Solution, stop when detecting solution to pH=7 with pH test paper；
(6) continue stirring 1 hour after forming colloid, close agitator, stand colloid and obtain colloid after 24 hours.
4. drying grinding colloid
(1) it is 90 DEG C by colloid oven for drying, temperature, 2.5 hours time, is dried into solid.It should be noted that it is Prevent colloid from splashing, initial temperature because less than 50 DEG C, being transferred to 90 DEG C again after the moisture evaporation in colloid；
(2) by solid abrasive 20min into powder.
5. cleaning
(1) powder is poured into deionized water and stirred, be completely dissolved the impurity in powder, stayed with filter paper sieve more pure Powder residue, wait natural air drying；
(2) by residue 300 DEG C of Muffle furnace process annealing 2 hours, 20min is fully ground in mortar；
(3) cleaning process is repeated 3 times.
4. annealing
Powder is put into Muffle furnace, 600 DEG C of annealing temperature, constant temperature 3 hours, it is required that cooling is taken out after 24 hours Al2O3- ZnO powder body materials.
5. gas sensor is made
(1) earthenware is welded on special pedestal, and by Al2O3- ZnO powder body materials and cetyl trimethyl bromine Change the ratio mixing of ammonium 4: 1, be then applied on earthenware, coating thickness 100um；
(2) obtained earthenware being put into process annealing 20min in horse expense stove, annealing temperature is 250 DEG C, constant temperature 10min, Take out to obtain gas sensor 2 after 24 hours
(3) its gas-sensitive property is determined with HW-30A type air-sensitive testers, show the gas sensor of the present invention has to acetone Very strong selectivity, it can exclude to measure the interference of other common organic steams in atmosphere.
6. aging
(1) gas sensor after test is inserted into desk-top gas sensor agingtable, is 5V in heating voltage, it is corresponding to add Hot temperature is 85 DEG C, under conditions of relative humidity is 50%RH, aging 6 days.
(2) its gas-sensitive property is determined with HW-30A type air-sensitive testers, gas sensor of the invention has very strong to acetone Selectivity and stability.
Embodiment 3：
1. prepare colloid
(1) configuration prepares the solvent of colloid.Absolute ethyl alcohol is mixed with deionized water according to 1: 1 volume ratio, stirred To uniform.
(2) Zn (CH are weighed respectively with electronic balance3COO)2·2H2O crystal and NaOH crystal, and respectively with preparing Solvent mixes, and obtained concentration is respectively 0.8mol/L and 1.6mol/L solution.
(3) w (Al are weighed with electronic balance2O3) be 5wt% Al (NO3)3·9H2O is mixed into Zn (CH3COO)2Solution In；
(4) by cetyl trimethylammonium bromide and Zn (CH3COO)2Solution is mixed with 1: 5 ratio；
(5) Zn (CH are stirred with mixer3COO)2Solution, rotating speed about 150r/min, by NaOH solution with 1ml/min drop Speed instills Zn (CH3COO)2Solution, stop when detecting solution to pH=7 with pH test paper；
(6) continue stirring 0.5 hour after forming colloid, close agitator, stand colloid and obtain colloid after 24 hours.
6. drying grinding colloid
(1) it is 80 DEG C by colloid oven for drying, temperature, 3 hours time, is dried into solid.It should be noted that in order to Prevent colloid from splashing, initial temperature because less than 50 DEG C, being transferred to 80 DEG C again after the moisture evaporation in colloid：
(2) by solid abrasive 20min into powder.
7. cleaning
(1) powder is poured into deionized water and stirred, be completely dissolved the impurity in powder, stayed with filter paper sieve more pure Powder residue, wait natural air drying；
(2) by residue 300 DEG C of Muffle furnace process annealing 1 hour, 20min is fully ground in mortar；
(3) cleaning process is repeated 3 times.
4. annealing
Powder is put into Muffle furnace, 800 DEG C of annealing temperature, constant temperature 2 hours, it is required that cooling is taken out after 24 hours Al2O3- ZnO powder body materials.
5. gas sensor is made
(1) earthenware is welded on special pedestal, and by Al2O3- ZnO powder body materials and cetyl trimethyl bromine Change the ratio mixing of ammonium 5: 1, be then applied on earthenware, coating thickness 50um；
(2) obtained earthenware is put into process annealing 30min in horse expense stove, annealing temperature is taken after being 250 DEG C, 24 hours Go out to obtain gas sensor；
(3) its gas-sensitive property is determined with HW-30A type air-sensitive testers, show the gas sensor of the present invention has to acetone Very strong selectivity, it can exclude to measure the interference of other common organic steams in atmosphere.
6. aging
(1) gas sensor after test is inserted into desk-top gas sensor agingtable, is 5.5V in heating voltage, it is corresponding Heating-up temperature is 99 DEG C, under conditions of relative humidity is 70%RH, aging 7 days.
(2) its gas-sensitive property is determined with HW-30A type air-sensitive testers, gas sensor of the invention still has to acetone Very strong selectivity and stability.

Claims (10)

1. a kind of preparation method of new high selectivity acetone gas sensor, process adulterates Zn (OH) to prepare2Colloid, colloid Drying grinding, cleaning, high annealing, powder coating process annealing and temperature and humidity control aging；It is characterized in that：Zn is adulterated preparing (OH)2During colloid, cetyl trimethylammonium bromide is added.
A kind of 2. preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that It is described to prepare doping Zn (OH)2The step of colloid process is：
Mixed using absolute ethyl alcohol with deionized water according to 1: 1-1: 2 volume ratio as solvent；
Use solvent Zn (CH3COO)2·2H2O crystal configuration Zn (CH3COO)2Solution；
In Zn (CH3COO)2Cetyl trimethylammonium bromide is added in solution；
In Zn (CH3COO)2Dopant Al (NO are added in solution3)3·9H2O；
Use solvent and NaOH configuration NaOH solutions；
In whipping process, the NaOH solution of configuration is instilled into Zn (CH3COO)2In solution, while pH value is monitored, when pH value reaches When 7, stop adding NaOH solution；
Continue agitating solution 0.5-1 hours；
Stand colloid and obtain colloid in 24 hours.
3. the preparation method of new high selectivity acetone gas sensor according to claim 1 or 2, it is characterised in that institute The preparation doping Zn (OH) stated2During colloid, Zn (CH3COO)2Solution molar concentration is 0.8-1mol/L, cetyl front three Base ammonium bromide adds Zn (CH with 1: 4-1: 5 volume ratio3COO)2In solution.
4. the preparation method of new high selectivity acetone gas sensor according to claim 1 or 2, it is characterised in that institute The preparation doping Zn (OH) stated2During colloid, in Zn (CH3COO)2Dopant Al (NO are added in solution3)3·9H2O doping Mass ratio is 4-5wt%.
5. the preparation method of new high selectivity acetone gas sensor according to claim 1 or 2, it is characterised in that institute The preparation doping Zn (OH) stated2During colloid, NaOH solution and the Zn (CH of configuration3COO)2The molar concentration ratio of solution is 2 : 1, NaOH solution instills Zn (CH3COO)2Drop speed in solution is 0.1-1ml/min, speed of agitator 80-150r/min.
6. the preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that described Colloid drying process of lapping, drying in an oven, temperature be 80-100 DEG C, hour time 2-3, be dried into solid；By solid Grind into powder, milling time 15-20 minutes.
7. the preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that described Cleaning process is filtered first to clean powder with deionized water with filter paper, and 300 DEG C of process annealing 1-2 are small in horse takes stove When, regrind powder 15-20 minutes；Cleaning process is in triplicate.
8. the preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that described High-temperature annealing process, it is by the 600-800 DEG C of annealing in horse takes stove of the powder after cleaning process, 2-3 hours.
9. the preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that described Powder coating process annealing process, it is uniformly to mix the powder after high annealing with cetyl trimethylammonium bromide, mixing Ratio is 4: 1-5: 1, is then coated with the middle part of earthenware (1) top layer (3), coating thickness 1-100um, is put into horse expense stove The process annealing 10-30 minutes of 250-300 DEG C of row, Al is made2O3The zno-based high selectivity acetone gas sensor of doping.
10. the preparation method of new high selectivity acetone gas sensor according to claim 1, it is characterised in that described Temperature and humidity control ageing process, temperature be 75-99 DEG C, relative humidity 30%-70%RH, ageing time 5-7 days.
CN201610819844.8A 2016-09-14 2016-09-14 The preparation method of new high selectivity acetone gas sensor Pending CN107817277A (en)

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Application publication date: 20180320