CN106290486B - A kind of New Co TiO3The preparation method and application of gas sensitive - Google Patents
A kind of New Co TiO3The preparation method and application of gas sensitive Download PDFInfo
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- CN106290486B CN106290486B CN201610583835.3A CN201610583835A CN106290486B CN 106290486 B CN106290486 B CN 106290486B CN 201610583835 A CN201610583835 A CN 201610583835A CN 106290486 B CN106290486 B CN 106290486B
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- 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
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Abstract
The invention discloses a kind of novel CoTiO3Gas sensitive, using cabaltous nitrate hexahydrate, tetra-n-butyl titanate as presoma, ethylene glycol monomethyl ether is solvent, and citric acid is complexing agent, respectively using polyethylene glycol, polypyrrole alkanone, cetyl trimethylammonium bromide as dispersing agent, CoTiO is prepared using sol-gel method3Nano material, and by CoTiO3Nano material is coated in the Al with Ag-Pd interdigital electrode2O3Plane gas sensitive device is fabricated on substrate.The CoTiO that the present invention makes3Gas sensitive device is quite fast to response/recovery time of ethyl alcohol, acetone gas, only about 15s, and sensitivity is higher, is a kind of novel gas sensitive.
Description
Technical field
The invention belongs to gas sensor technical fields, add a variety of dispersions when using sol-gal process nano material grown
Agent changes the specific surface area of nano material, to obtain highly sensitive novel gas sensitive.
Background technique
With the improvement of living standards, environmental pollution increasingly deteriorates.Not only atmosphere is contaminated, but also indoor environment
It is heavily contaminated.The measure of responding actively is taken to prevent in order to predict gas pollutant in today of science and technology and productivity dynamics
Or gaseous contamination is reduced, it explores novel gas sensitive material and is undoubtedly a long-term task.In order to improve semiconductor gas
The sensitivity of body sensor, researcher do various trial work, such as doping vario-property, and the measures such as addition dispersing agent, complexing agent improve
Air-sensitive performance.
Since nano material has many advantages, such as large specific surface area, small-size effect, traditional material is prepared into formation of nanostructured
It can get excellent performance.By the nanosizing of semiconductor oxide materials, low-dimensional, the gas sensing property of material can be improved；And it will be from
Sub- crystalline oxide material nanosizing, low-dimensional even can find it with excellent gas sensing property sometimes.
CoTiO3Belong to trigonal system, ilmenite crystal.Its structure is by corundum Al2O3It is derived, Co2+And Ti4+Respectively
Replace the Al in corundum structure3+Ion, and Co layers and Ti layers are alternately arranged to form rhombohedral structure.It has excellent mechanicalness
The performances such as energy, thermal stability, weak magnetic, weak semiconductive, low-k are a kind of new function materials.In addition, nanometer
CoTiO3Excellent sensitlzing effect is also shown, such as air-sensitive and light sensitive effect.
Currently, preparation CoTiO3The method of nano material is relatively more, there is sol-gal process, hydro-thermal method, chemical coprecipitation
Deng.To acquisition particle size, small, large specific surface area nano particle, sol-gal process prepare CoTiO3Nano material is one
Kind is cheap, can be realized the wet chemical method for preparing material of large-scale production.It is prepared in the present invention using sol-gal process
CoTiO3Nano material has response time and recovery time fast, is a kind of excellent gas sensitive.
Summary of the invention
Goal of the invention: a kind of excellent it is an object of the invention to find to solve the technical problems existing in the prior art
CoTiO3Gas sensitive improves sensitivity, response time and the recovery time of material.
Technical solution: to realize the above-mentioned technical purpose, the present invention provides a kind of CoTiO3Gas sensitive, the air-sensitive
For material using ethylene glycol monomethyl ether as solvent, citric acid is complexing agent, and utilizes polyethylene glycol, polypyrrole alkanone and cetyl front three
Any one in base ammonium bromide is prepared as dispersing agent using sol-gal process.
Present invention further proposes above-mentioned CoTiO3The preparation method of gas sensitive, includes the following steps:
(1) tetra-n-butyl titanate of 0.01mol is instilled into 50ml ethylene glycol monomethyl ether solution with 10~30 drops/min speed
In, after dissolution is sufficiently stirred, the cabaltous nitrate hexahydrate of 0.01mol is added into mixed solution, obtains royal purple solution, solution
Concentration about 0.2mol/L, Co in solution2+∶Ti4+=1: 1~1.05；
(2) it weighs monohydrate potassium to be added in the royal purple solution that step (1) obtains, after dissolution is sufficiently stirred, obtain
To transparent royal purple solution, citric acid and cation mole number ratio are 1: 1~4 in solution, and the cation refers to Co2+
And Ti4+Summation；
(3) dispersing agent is added in the solution obtained to step (2), is sufficiently stirred, obtains colloidal sol；
(4) after standing obtained colloidal sol, freeze-day with constant temperature in an oven is put, xerogel is obtained, xerogel is placed in agate
It is fully ground in mortar, obtains dry gel powder；
(5) xerogel is subjected to first time calcining, obtains black or blackish green powder；Again by the black of pre-burning or blackish green
Powder, which is put into sintering furnace, carries out second of calcining, then cools to room temperature with the furnace, obtains CoTiO3Nano material.
Preferably, in step (1), the dispersing agent is cetyl trimethylammonium bromide, polypyrrole alkanone and poly- second
Any one in glycol, dosage is about 0.1~0.15g.
In step (4), time of repose is 12h~48h.
In step (4), for 24 hours~48h is dried when the condition of freeze-day with constant temperature is 90 DEG C~120 DEG C.
It is further preferred that sol body is placed in 90 DEG C of freeze-day with constant temperature 12h first, then be warming up to 120 DEG C in step (4)
Freeze-day with constant temperature for 24 hours, obtains cellular xerogel.
In step (5), the condition of calcining is 350 DEG C~450 DEG C calcinings 3~6 hours for the first time, removes hydrone, second two
Alcohol methyl ether, citric acid organic matter, cobalt nitrate and tetra-n-butyl titanate decomposition product.The condition of second calcining be 500 DEG C~
700 DEG C of warm areas are calcined 3~6 hours, and CoTiO is obtained3Nano material.
Present invention further proposes above-mentioned CoTiO3Application of the material in production gas sensitive device.
Specifically, in the production process, CoTiO is taken3Nano material is slurred material with deionized water, then uniformly coating
In the plane Al for having Ag-Pd interdigital electrode2O3On substrate, dry in the shade to obtain CoTiO in air3Gas sensitive device.
The utility model has the advantages that compared with prior art, the present invention has the advantage that
(1) for the first time by CoTiO3Nano material is fabricated to plane gas sensitive device, has to steam such as ethyl alcohol, acetone higher
Sensitivity and quick response speed, response time only about 15s, to the ethyl alcohol of 100ppm, high sensitivity is up to 55.
(2) present invention prepares CoTiO using sol-gal process3Nano material realizes it in plane gas sensitive device for the first time
The application of aspect is suitble to the gas sensitive device of production small size.
Detailed description of the invention
Fig. 1 is the hot weight-differential heat curve of xerogel of the present invention；
Fig. 2 is CoTiO of the present invention3The XRD diagram of material；
Fig. 3 is CoTiO of the present invention3Gas sensitive device is to the ethyl alcohol of 50ppm and the sensitivity temperature curve of acetone；
Fig. 4 is CoTiO of the present invention3Sensitivity Time curve of the gas sensitive device to different concentration ethanol and acetone.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Embodiment will be helpful to those skilled in the art
Further understand the present invention.It should be pointed out that the present invention is for the first time by CoTiO3Application of micron in plane gas sensitive device,
Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Embodiment
Present embodiments provide CoTiO3The preparation method and gas sensing property of nano material, the specific steps are as follows:
A) tetra-n-butyl titanate for weighing 0.01mol is slowly dropped into the ethylene glycol monomethyl ether solvent of 50ml, and magnetic agitation makes
It is sufficiently dissolved.The cabaltous nitrate hexahydrate for weighing 0.01mol is added in mixed solution, is sufficiently stirred to obtain royal purple molten
Liquid weighs the monohydrate potassium of 0.02mol, is added in royal purple solution, weighs the cetyl trimethyl bromine of 0.1g
Change ammonium dispersing agent (CTAB) to be added in solution, obtains transparent mixed solution.Solution concentration is about 0.2mol/L, in solution
Co2+And Ti4+The ratio of ion is 1: 1, metal cation (Co2+And Ti4+Summation) it with the molar ratio of citric acid is 1: 1.
B) it stands to be put into afterwards for 24 hours in baking oven and be dried for 24 hours in 90 DEG C；Then it is dried for 24 hours at 120 DEG C, obtains cellular xerogel.
After being cooled to room temperature, xerogel is placed in mortar and grinds about 20min, obtains dry gel powder.
It is as shown in Figure 1 CoTiO in the present embodiment3The hot weight-differential heat curve of xerogel.As seen from the figure: xerogel is 30
DEG C~120 DEG C of warm areas, weight loss about 10%, caused by the water vapour evaporation mainly in xerogel；In 120 DEG C~400 DEG C temperature
Area, weight loss about 80%, the mainly combustion decomposition of organic matter and nitrate；In 400 DEG C~550 DEG C warm areas, weight loss
Seldom, mainly organic matter mostly burns completely.In 550 DEG C or more warm areas, weight is increased slightly, it may be possible to CoTiO3It crystallized
The process that a small amount of oxygen in air generates crystal is absorbed in journey.In differential thermal curve, 250 DEG C, 300 DEG C of exothermic peaks correspond respectively to
The decomposition temperature of citric acid and ethylene glycol monomethyl ether；The burning that 380 DEG C of exothermic peaks correspond to citric acid network collapses, and releases a large amount of
Heat；580 DEG C of endothermic peaks correspond to CoTiO3Crystallization process heat absorption.It follows that CoTiO3Crystallization temperature should be higher than that 580 DEG C or more.
C) CoTiO is arranged according to thermogravimetric differential thermal curve3The temperature curve of material, with the heating rate of 2 DEG C/min from room temperature
450 DEG C are risen to, in 450 DEG C of heat preservation 6h, room temperature is down to the rate (about 1 DEG C/min) of Temperature fall in air, pre-burning removal is big
Black or blackish green CoTiO are obtained after partial organic substances3Powder.By the CoTiO of pre-burning3After powder mull about 20min, with 2
DEG C/heating rate of min rises to 700 DEG C from room temperature, in 700 DEG C of heat preservation 6h, and 400 are cooled to the rate of temperature fall of 2 DEG C/min
DEG C, from 400 DEG C to room temperature, room temperature is down to the rate (about 1 DEG C/min) of Temperature fall in air, obtains CoTiO3Nanometer material
Material.
Fig. 2 is shown: after addition CTAB dispersing agent, the CoTiO through pre-burning3Powder CoTiO made of 700 DEG C of sintering3Material
Corresponding XRD curve.As seen from the figure, the CoTiO being sintered at such a temperature3Nano material is a kind of single-phase tripartite without miscellaneous phase
Crystallographic system ilmenite crystal structure materials.
Fig. 3 is the CoTiO prepared in the present embodiment in 700 DEG C3Powder is the spirit of 50ppm ethyl alcohol, acetone steam to concentration
Sensitivity temperature curve.As seen from the figure: the CoTiO of 700 DEG C of preparations3Powder has best spirit when gas sensitive device temperature is 240 DEG C
Sensitivity, the i.e. operating temperature of the gas sensitive device are 240 DEG C.
Fig. 4 is the CoTiO prepared in the present embodiment in 700 DEG C3Powder is in operating temperature to different concentration ethanol steam
The Sensitivity Time curve tested at 240 DEG C.As seen from the figure: CoTiO3It is very fast to the response speed of ethyl alcohol and acetone steam,
About 15s, can be beautiful compared with the response time of the gas sensitives such as the ZnO for having been carried out industrial application.
The foregoing is merely one embodiment of the present invention, it is not all of or unique embodiment, this field is common
Any equivalent improvement that technical staff takes technical solution of the present invention by reading description of the invention, is of the invention
Claim is covered.
Claims (6)
1. a kind of CoTiO3The preparation method of gas sensitive, which is characterized in that the gas sensitive is molten with ethylene glycol monomethyl ether
Agent, citric acid are complexing agent, and utilize any one in polyethylene glycol, polypyrrole alkanone and cetyl trimethylammonium bromide
It as dispersing agent, is prepared, is included the following steps: using sol-gal process
(1) tetra-n-butyl titanate is instilled in ethylene glycol monomethyl ether solvent with 10~30 drops/min speed, after dissolution is sufficiently stirred,
Cabaltous nitrate hexahydrate is added into solution, obtains royal purple solution, solution concentration about 0.2mol/L, Co in solution2+:Ti4+=
1:1~1.05；
(2) it weighs monohydrate potassium to be added in the royal purple solution that step (1) obtains, wherein citric acid rubs with cation
Your number ratio is 1:1~4, and the cation refers to Co2+And Ti4+Summation；
(3) dispersing agent is added in the solution obtained to step (2), is sufficiently stirred, obtains sol body；
(4) after standing obtained sol body, freeze-day with constant temperature in an oven is put, xerogel is obtained, xerogel is placed in agate and is ground
It is fully ground in alms bowl, obtains dry gel powder；
(5) dry gel powder is subjected to first time calcining, obtains black or blackish green powder；Again by the black of pre-burning or blackish green
Powder, which is put into sintering furnace, carries out second of calcining, then cools to room temperature with the furnace, obtains CoTiO3Nano material；
Wherein, the dispersing agent is any one in cetyl trimethylammonium bromide, polypyrrole alkanone and polyethylene glycol,
Dosage is 0.1 ~ 0.15g；In step (5), the condition of calcining is 350 DEG C ~ 450 DEG C calcinings 3 ~ 6 hours for the first time, removes moisture removal
Son, ethylene glycol monomethyl ether, citric acid network, cobalt nitrate and tetra-n-butyl titanate decomposition product；Second of calcination condition is at 500 DEG C
~ 700 DEG C of warm areas are calcined 3 ~ 6 hours, and CoTiO is obtained3Nanocrystalline material.
2. preparation method according to claim 1, which is characterized in that in step (4), time of repose is 12h ~ 48h.
3. preparation method according to claim 1, which is characterized in that in step (4), the condition of freeze-day with constant temperature is 90 DEG C~
At 120 DEG C freeze-day with constant temperature for 24 hours ~ 48h.
4. preparation method according to claim 1, which is characterized in that in step (4), sol body is placed in 90 DEG C of perseverances first
The dry 12h of temperature, then it is warming up to 120 DEG C of freeze-day with constant temperature for 24 hours, obtain cellular xerogel.
5. the CoTiO that preparation method described in claim 1 is prepared3Application of the material in production gas sensitive device.
6. application according to claim 5, which is characterized in that in the production process, by CoTiO3Nano material uniformly coats
In the plane Al for having Ag-Pd interdigital electrode2O3On substrate, drying in the shade in air can be obtained CoToO3Gas sensitive device.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110104678B (en) * | 2019-05-16 | 2021-10-08 | 沈阳工业大学 | Cobalt titanate gas-sensitive material with high sensitivity to low-concentration ethanol and preparation method thereof |
| CN111992257B (en) * | 2020-03-25 | 2024-02-13 | 武汉纺织大学 | Modified perovskite hollow porous microsphere for catalytic degradation of antibiotics, and preparation method and application thereof |
| CN111537585A (en) * | 2020-04-17 | 2020-08-14 | 江苏奥力威传感高科股份有限公司 | Based on YSZ and CoTiO3Mixed potential type NO of sensitive electrode2Sensor, preparation method and application thereof |
| CN113238005B (en) * | 2021-05-12 | 2024-01-23 | 深圳万知达科技有限公司 | N/CoTiO with alcohol-sensitive aldehyde-sensitive dual functions 3 @g-C 3 N 4 Composite material, preparation method and application thereof |
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| CN101493430A (en) * | 2009-02-17 | 2009-07-29 | 武汉工程大学 | Hydrogen sulfide gas sensitive, preparation, and method for making hydrogen sulfide gas sensitive device |
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| CN101493430A (en) * | 2009-02-17 | 2009-07-29 | 武汉工程大学 | Hydrogen sulfide gas sensitive, preparation, and method for making hydrogen sulfide gas sensitive device |
| CN105203598B (en) * | 2015-10-08 | 2018-04-06 | 江苏科技大学 | A kind of bismuth ferrite gas sensitive of quick response and its application |
| CN105259214A (en) * | 2015-10-31 | 2016-01-20 | 武汉工程大学 | Toluene and xylene gas sensitive material and preparation thereof as well as preparation method of toluene and xylene gas sensitive device |
Non-Patent Citations (1)
| Title |
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| 敏感型CoTi0<sub/>3</sub>微晶及薄膜的制备、结构和性能研究;卢靖;《万方数据》;20121231;12、44-52、89 |
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