CN108609667A - Ozone gas sensitive and preparation method, ozone gas sensitive device and preparation method - Google Patents
Ozone gas sensitive and preparation method, ozone gas sensitive device and preparation method Download PDFInfo
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- CN108609667A CN108609667A CN201810532248.0A CN201810532248A CN108609667A CN 108609667 A CN108609667 A CN 108609667A CN 201810532248 A CN201810532248 A CN 201810532248A CN 108609667 A CN108609667 A CN 108609667A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention relates to a kind of ozone gas sensitive and preparation method thereof and ozone gas sensitive devices and preparation method thereof.Ozone gas sensitive is Co3O4It is 100~250nm that nano-powder, which is hollow cube structure and its grain size,.Gas sensitive preparation method is：Stannic chloride aqueous solution and aqueous citric acid solution are mixed to get solution I；Cobalt chloride solution is mixed with solution I, NaOH or KOH stirrings are added, and addition NaOH or KOH stirs to get mixed solution again, and the NaOH or the molar ratio of KOH and stannic chloride being added for the first time and for the second time are respectively 6~10:1 and 30~50:1；Mixed solution is subjected to hydro-thermal reaction and filters reaction product, is washed, is dry, obtain presoma and presoma heating calcining is obtained into Co3O4Nano-powder.Gas sensitive of the present invention is good to high sensitivity, the selectivity of ozone, and the gas sensitive device of preparation has the detection function highly sensitive to ozone gas.
Description
Technical field
The present invention relates to Semiconductor gas sensors original paper technical fields, and in particular to a kind of ozone gas sensitive and its preparation and
Ozone gas sensitive device and preparation method thereof.
Background technology
Ozone is a kind of oxidant, and the ozone of low concentration can play the role of purification, sterilization to air, but when indoor
Ozone concentration is higher than 0.1mg/m3When can cause air pollution and certain harm is generated to health, it will usually there is skin thorn
Itch, unsmooth breath, the symptoms such as cough and rhinitis, and also Central nervous system, eyes also have stimulation, can also draw when serious
Asthma, pulmonary emphysema etc. are sent out, therefore it is most important to detect ozone concentration.
Currently, the detection method of ozone includes mainly：Iodimetric titration, ultraviolet-visible absorption photometry, chemoluminescence method, electricity
Sub- spin resonance method, high performance liquid chromatography, semiconductor gas sensor etc..However, iodimetric titration easily by its oxidant such as NO,
The interference of the substances such as Cl2；The remolding sensitivity of ultraviolet-visible absorption photometry is relatively low；Chemoluminescence method selects judging from the current situation
Selecting property is poor；The instrument price of electron spin resonance is expensive, is not suitable for public use；High performance liquid chromatography compares other skills
Art means operating procedure is various；Compared with above several detection methods, semiconductor gas sensor just show it is easy to operate,
High sensitivity, selectively single-minded etc. advantages.
The performance of ozone semiconductor gas sensor depends primarily on the performance of gas sensitive.Not maturation domestic at present
Ozone gas sensitive, therefore prepare that a kind of response sensitivity is high, operating temperature is low, ultralow detectable limit and long-time stability are good
Ozone gas sensitive and its gas sensor will have prodigious market prospects.
Invention content
Technical problem to be solved by the invention is to provide a kind of high sensitivity, selectivity is good, operating temperature is low, long-term steady
The preparation method of qualitative good ozone gas sensitive and preparation method thereof and ozone gas sensitive device.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
A kind of ozone gas sensitive is provided, the ozone gas sensitive is Co3O4Nano-powder, the Co3O4Nano-powder
It is 100~250nm for hollow cube structure and its grain size.
The preparation method for providing above-mentioned ozone gas sensitive, includes the following steps：
(1) SnCl is weighed4·5H2O is configured to stannic chloride aqueous solution, weighs citric acid and is configured to aqueous citric acid solution, by two
Kind solution, which is uniformly mixed, obtains solution I；
(2) by CoCl2·6H2O is soluble in water, obtains solution II；
(3) under magnetic stirring the solution I and the solution II are mixed and stirred for uniformly, NaOH or KOH being added, stirs
Mix 15-30min, then second NaOH or KOH be added, stir 15min, obtain mixed solution, the NaOH being added for the first time or
The molar ratio of KOH and stannic chloride in mixed solution is 6~10:1, second of NaOH being added or KOH and chlorination in mixed solution
The molar ratio of tin is 30~50:1；
(4) mixed solution is transferred in reaction kettle and carries out hydro-thermal reaction, after reaction, reaction product is filtered,
Washing, drying, obtain presoma cobalt hydroxide nano-powder；
(5) the presoma cobalt hydroxide nano powder is subjected to heating calcining and obtains the Co3O4Nano-powder is as smelly
Oxygen gas sensitive.
Further, SnCl in the solution I4·5H2The concentration of O and citric acid is 0.1-0.4mol/L.
Further, SnCl in the mixed solution4·5H2O and CoCl2·6H2The molar ratio of O is 1:1.
Further, the reaction temperature of the hydro-thermal reaction is 120-200 DEG C, reaction time 8-14h.
Further, the temperature calcined in the step (5) is 300 DEG C, time 1-4h.
The present invention provides the ozone gas sensitive device that above-mentioned ozone air-sensitive material preparation obtains.
The present invention also provides the preparation methods of above-mentioned ozone gas sensitive device, include the following steps：By the ozone air-sensitive material
It is mixed with absolute ethyl alcohol after abrasive lapping and is tuned into paste, by its even application through annealing after electrode pipe surface, natural air drying
Obtain gas sensing electrode pipe, then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, system
It is standby to obtain ozone gas sensitive device.
Further, the temperature of the annealing is 300~450 DEG C, and the time is 0.5~4h.
The key technical indexes of ozone gas sensitive device of the present invention is as follows：
1, the detection range of device：10ppm-10000ppm (gas volume fractions：1ppm=1X10-6)；
2, the operating temperature of device：25℃-300℃；
3, detection sensitivity：3-500；
4, the device reaction time：Less than 60s；
5, device recovery time：Less than 60s.
The beneficial effects of the invention are as follows：The present invention has synthesized a kind of novel semi-conductor gas sensitive, novel is partly led with this
The ozone gas sensitive device that body material makes has the detection function highly sensitive to ozone gas, to the ozone gas of 100ppm concentration
Body sensitivity can be used for the safety detection of ozone in air in 90-150,.And the ozone gas sensitive device that the present invention makes has
Higher selectivity, (ozone sensitivity relatively low to the sensitivity of n-butanol, dimethylbenzene, formaldehyde：N-butanol sensitivity=12:1,
Ozone sensitivity：Dimethylbenzene sensitivity=13:1, ozone sensitivity：Formaldehyde sensitivity=40:1), only have to ozone higher
Sensitivity.
Description of the drawings
Fig. 1 is the Co that the embodiment of the present invention 1 obtains3O4Transmission electron microscope picture；
Specific implementation mode
Principles and features of the present invention are described below in conjunction with drawings and the specific embodiments, example is served only for solving
The present invention is released, is not intended to limit the scope of the present invention.
Embodiment 1
The preparation of ozone gas sensitive device
(1) 35.06g (0.1mol) SnCl is weighed4·5H2O is dissolved in 1L water, by 21.0g (0.1mol) C8H8O7·H2O is molten
In 1L water, two kinds of solution are uniformly mixed and obtain solution I；
(2) by 23.80g (0.2mol) CoCl2·6H2O is dissolved in 1L water, obtains solution II；
(3) solution I and the solution II are mixed and stirred under magnetic stirring uniformly, the NaOH of 1L0.6mol/L being added
Solution stirs 15-30min, and the NaOH solution stirring 15min that 1L 3mol/L are added obtains mixed solution, then mixes gained
Solution, which is transferred in reaction kettle, carries out solvent thermal reaction, and 12h is reacted at 180 DEG C, will be anti-then by reaction kettle cooled to room temperature
It answers product to filter, wash, is dry, obtaining presoma cobalt hydroxide nano-powder.
4) obtained presoma cobalt hydroxide nano-powder is put into Muffle furnace to the 300 DEG C of calcinings that heat up to obtain for 4 hours
Co3O4Nano-powder, as ozone gas sensitive.The present embodiment products therefrom is subjected to phenetic analysis, result is hollow cube
Body structure, purity are more than 99%, average grain diameter 120nm.
5) Co obtained above is weighed3O4Nano-powder 1g fine gtindings, are used in combination appropriate absolute ethyl alcohol to be tuned into paste, then
Its even application is obtained into gas sensing electrode pipe after electrode pipe surface, natural air drying through 300~450 DEG C of 0.5~4h of annealing,
Then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, ozone sensor for gas is prepared
Part.
The ozone gas sensitive device that the present embodiment is prepared uses the air-sensitive of Zhengzhou Wei Sheng Electronic Technology Co., Ltd's production
Element test system WS-30A instruments carry out air-sensitive performance test, and test method is static volumetric method.Test result is：Work as work
When temperature is 100 DEG C, the sensitivity to 100ppm ozone is 140, the sensitivity shown to ozone.
Embodiment 2
The preparation of ozone gas sensitive device
(1) 1.052g (3mmol) SnCl is weighed4·5H2O is dissolved in 10mL water, by 0.63g (3mmol) C8H8O7·H2O is molten
In 10mL water, two kinds of solution are uniformly mixed and obtain solution I；
(2) by 0.7138g (3mmol) CoCl2·6H2O is dissolved in 10mL water, obtains solution II；
(3) solution I and the solution II are mixed and stirred under magnetic stirring uniformly, the NaOH of 10mL3mol/L being added
Solution stirs 15-30min, and the NaOH solution stirring 15min that 20mL 7.5mol/L are added obtains mixed solution, then by gained
Mixed solution, which is transferred in reaction kettle, carries out solvent thermal reaction, and 8h is reacted at 200 DEG C, then by reaction kettle cooled to room temperature,
Reaction product is filtered, is washed, is dry, obtains presoma cobalt hydroxide nano-powder.
4) obtained presoma cobalt hydroxide nano-powder is put into Muffle furnace to the 300 DEG C of calcinings that heat up to obtain for 2 hours
Co3O4Nano-powder, as ozone gas sensitive.The present embodiment products therefrom is subjected to phenetic analysis, result is hollow cube
Body structure, purity are more than 99%, average grain diameter 210nm.
5) Co obtained above is weighed3O4Nano-powder 1g fine gtindings, are used in combination appropriate absolute ethyl alcohol to be tuned into paste, then
Its even application is obtained into gas sensing electrode pipe after electrode pipe surface, natural air drying through 300~450 DEG C of 0.5~4h of annealing,
Then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, ozone sensor for gas is prepared
Part.
The ozone gas sensitive device that the present embodiment is prepared uses the air-sensitive of Zhengzhou Wei Sheng Electronic Technology Co., Ltd's production
Element test system WS-30A instruments carry out air-sensitive performance test, and test method is static volumetric method.Test result is：Work as work
When temperature is 100 DEG C, the sensitivity to 100ppm ozone is 110, the sensitivity shown to ozone.
Embodiment 3
The preparation of ozone gas sensitive device
(1) 2.805g (8mmol) SnCl is weighed4·5H2O is dissolved in 20mL water, by 1.680g (8mmol) C8H8O7·H2O
It is dissolved in 20mL water, two kinds of solution is uniformly mixed and obtain solution I；
(2) by 1.903g (8mmol) CoCl2·6H2O is dissolved in 20mL water, obtains solution II；
(3) solution I and the solution II are mixed and stirred under magnetic stirring uniformly, being added 20mL3.6mol/L's
NaOH solution stirs 15-30min, and the NaOH solution stirring 15min that 40mL 7.2mol/L are added obtains mixed solution, then will
Gained mixed solution, which is transferred in reaction kettle, carries out solvent thermal reaction, and 8h is reacted at 120 DEG C, reaction kettle is then naturally cooled to room
Reaction product is filtered, is washed, is dry, obtaining presoma cobalt hydroxide nano-powder by temperature.
4) obtained presoma cobalt hydroxide nano-powder is put into Muffle furnace to the 300 DEG C of calcinings that heat up to obtain for 1 hour
Co3O4Nano-powder, as ozone gas sensitive.The present embodiment products therefrom is subjected to phenetic analysis, result is hollow cube
Body structure, purity are more than 99%, average grain diameter 250nm.
5) Co obtained above is weighed3O4Nano-powder 1g fine gtindings, are used in combination appropriate absolute ethyl alcohol to be tuned into paste, then
Its even application is obtained into gas sensing electrode pipe after electrode pipe surface, natural air drying through 300~450 DEG C of 0.5~4h of annealing,
Then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, ozone sensor for gas is prepared
Part.
The ozone gas sensitive device that the present embodiment is prepared uses the air-sensitive of Zhengzhou Wei Sheng Electronic Technology Co., Ltd's production
Element test system WS-30A instruments carry out air-sensitive performance test, and test method is static volumetric method.Test result is：Work as work
When temperature is 100 DEG C, the sensitivity to 100ppm ozone is 90, the sensitivity shown to ozone.
Embodiment 4
The preparation of ozone gas sensitive device
(1) 1.4kg (4mol) SnCl is weighed4·5H2O is dissolved in 20L water, by 840g (4mol) C8H8O7·H2O is dissolved in 20L
In water, two kinds of solution are uniformly mixed and obtain solution I；
(2) by 951.72g (4mol) CoCl2·6H2O is dissolved in 20L water, obtains solution II；
(3) solution I and the solution II are mixed and stirred under magnetic stirring uniformly, being added 20L1.8mol/L's
NaOH solution stirs 15-30min, and the NaOH solution stirring 15min that 20L 8mol/L are added obtains mixed solution, then by gained
Mixed solution, which is transferred in reaction kettle, carries out solvent thermal reaction, and 8h is reacted at 120 DEG C, then by reaction kettle cooled to room temperature,
Reaction product is filtered, is washed, is dry, obtains presoma cobalt hydroxide nano-powder.
4) obtained presoma cobalt hydroxide nano-powder is put into Muffle furnace to the 300 DEG C of calcinings that heat up to obtain for 2 hours
Co3O4Nano-powder, as ozone gas sensitive.The present embodiment products therefrom is subjected to phenetic analysis, result is hollow cube
Body structure, purity are more than 99%, average grain diameter 100nm.
5) Co obtained above is weighed3O4Nano-powder 1g fine gtindings, are used in combination appropriate absolute ethyl alcohol to be tuned into paste, then
Its even application is obtained into gas sensing electrode pipe after electrode pipe surface, natural air drying through 300~450 DEG C of 0.5~4h of annealing,
Then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, ozone sensor for gas is prepared
Part.
The ozone gas sensitive device that the present embodiment is prepared uses the air-sensitive of Zhengzhou Wei Sheng Electronic Technology Co., Ltd's production
Element test system WS-30A instruments carry out air-sensitive performance test, and test method is static volumetric method.Test result is：Work as work
When temperature is 100 DEG C, the sensitivity to 100ppm ozone is 150, the sensitivity shown to ozone.
Embodiment 5
The preparation of ozone gas sensitive device
(1) 175.3g (0.5mol) SnCl is weighed4·5H2O is dissolved in 2L water, by 105g (0.5mol) C8H8O7·H2O is molten
In 2L water, two kinds of solution are uniformly mixed and obtain solution I；
(2) by 118.97g (0.5mol) CoCl2·6H2O is dissolved in 2L water, obtains solution II；
(3) solution I and the solution II are mixed and stirred for uniformly under magnetic stirring, the NaOH that 2L2mol/L is added is molten
Liquid stirs 15-30min, and the NaOH solution stirring 15min that 2L 7.5mol/L are added obtains mixed solution, then mixes gained
Solution, which is transferred in reaction kettle, carries out solvent thermal reaction, and 14h is reacted at 150 DEG C, will be anti-then by reaction kettle cooled to room temperature
It answers product to filter, wash, is dry, obtaining presoma cobalt hydroxide nano-powder.
4) obtained presoma cobalt hydroxide nano-powder is put into Muffle furnace to the 300 DEG C of calcinings that heat up to obtain for 2 hours
Co3O4Nano-powder, as ozone gas sensitive.The present embodiment products therefrom is subjected to phenetic analysis, result is hollow cube
Body structure, purity are more than 99%, average grain diameter 200nm.
5) Co obtained above is weighed3O4Nano-powder 1g fine gtindings, are used in combination appropriate absolute ethyl alcohol to be tuned into paste, then
Its even application is obtained into gas sensing electrode pipe after electrode pipe surface, natural air drying through 300~450 DEG C of 0.5~4h of annealing,
Then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft, voltage ageing, encapsulation, ozone sensor for gas is prepared
Part.
The ozone gas sensitive device that the present embodiment is prepared uses the air-sensitive of Zhengzhou Wei Sheng Electronic Technology Co., Ltd's production
Element test system WS-30A instruments carry out air-sensitive performance test, and test method is static volumetric method.Test result is：Work as work
When temperature is 100 DEG C, the sensitivity to 100ppm ozone is 123, the sensitivity shown to ozone.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of ozone gas sensitive, which is characterized in that the ozone gas sensitive is Co3O4Nano-powder, the Co3O4Nanometer
Powder is hollow cube structure and its grain size is 100~250nm.
2. a kind of preparation method of ozone gas sensitive as described in claim 1, which is characterized in that include the following steps：
(1) SnCl is weighed4·5H2O is configured to stannic chloride aqueous solution, weighs citric acid and is configured to aqueous citric acid solution, molten by two kinds
Liquid is uniformly mixed and obtains solution I；
(2) by CoCl2·6H2O is soluble in water, obtains solution II；
(3) solution I and the solution II are mixed and stirred under magnetic stirring uniformly, NaOH or KOH, stirring being added
Then 15-30min is added NaOH or KOH second, stirs 15min, obtain mixed solution, the NaOH or KOH being added for the first time
Molar ratio with stannic chloride in mixed solution is 6~10:1, second of NaOH being added or KOH and stannic chloride in mixed solution
Molar ratio is 30~50:1；
(4) mixed solution is transferred in reaction kettle and carries out hydro-thermal reaction, after reaction, reaction product is filtered, is washed,
It is dry, obtain presoma cobalt hydroxide nano-powder；
(5) the presoma cobalt hydroxide nano powder is subjected to heating calcining and obtains the Co3O4Nano-powder, as ozone gas
Quick material.
3. the preparation method of ozone gas sensitive according to claim 2, which is characterized in that SnCl in the solution I4·
5H2The concentration of O and citric acid is 0.1~0.4mol/L.
4. the preparation method of ozone gas sensitive according to claim 2, which is characterized in that in the mixed solution
SnCl4·5H2O and CoCl2·6H2The molar ratio of O is 1:1.
5. a kind of preparation method of gas sensitive according to claim 2, which is characterized in that the reaction of the hydro-thermal reaction
Temperature is 120~200 DEG C, and the reaction time is 8~14h.
6. the preparation method of ozone gas sensitive according to claim 2, which is characterized in that calcining in the step (5)
Temperature be 300~500 DEG C, the time be 1~4h.
7. a kind of ozone gas sensitive device, which is characterized in that obtained using ozone air-sensitive material preparation described in claim 1.
8. a kind of preparation method of ozone gas sensitive device as claimed in claim 7, which is characterized in that include the following steps：It will
It is mixed with absolute ethyl alcohol after the ozone gas sensitive grinding and is tuned into paste, by its even application in electrode pipe surface, natural wind
Gas sensing electrode pipe is obtained through annealing after dry, then gas sensing electrode pipe is welded according to heater-type structure traditional handicraft,
Ozone gas sensitive device is prepared in voltage ageing, encapsulation.
9. the preparation method of ozone gas sensitive device according to claim 8, which is characterized in that the temperature of the annealing
It it is 300~450 DEG C, the time is 0.5~4h.
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| CN110455874A (en) * | 2019-08-22 | 2019-11-15 | 有研工程技术研究院有限公司 | A kind of CoSn double metal oxide semiconductor material and preparation method thereof |
| CN110672669A (en) * | 2019-10-14 | 2020-01-10 | 武汉工程大学 | Cobaltosic oxide gas-sensitive device, preparation method and application thereof, and ozone-assisted n-butanol gas testing method |
| CN111024775A (en) * | 2018-10-09 | 2020-04-17 | 中国科学院物理研究所 | Gas-sensitive sensing device for ozone gas sensor and preparation method |
| CN114577862A (en) * | 2022-02-16 | 2022-06-03 | 中国科学院合肥物质科学研究院 | Ozone gas sensor and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024775A (en) * | 2018-10-09 | 2020-04-17 | 中国科学院物理研究所 | Gas-sensitive sensing device for ozone gas sensor and preparation method |
| CN111024775B (en) * | 2018-10-09 | 2021-05-25 | 中国科学院物理研究所 | Gas-sensitive sensing device for ozone gas sensor and preparation method |
| CN110455874A (en) * | 2019-08-22 | 2019-11-15 | 有研工程技术研究院有限公司 | A kind of CoSn double metal oxide semiconductor material and preparation method thereof |
| CN110672669A (en) * | 2019-10-14 | 2020-01-10 | 武汉工程大学 | Cobaltosic oxide gas-sensitive device, preparation method and application thereof, and ozone-assisted n-butanol gas testing method |
| CN110672669B (en) * | 2019-10-14 | 2022-03-29 | 武汉工程大学 | Cobaltosic oxide gas-sensitive device, preparation method and application thereof, and ozone-assisted n-butanol gas testing method |
| CN114577862A (en) * | 2022-02-16 | 2022-06-03 | 中国科学院合肥物质科学研究院 | Ozone gas sensor and preparation method and application thereof |
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