CN108508065A - A kind of order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of ultra-fine skeleton and preparation method thereof - Google Patents
A kind of order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of ultra-fine skeleton and preparation method thereof Download PDFInfo
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- CN108508065A CN108508065A CN201810286398.8A CN201810286398A CN108508065A CN 108508065 A CN108508065 A CN 108508065A CN 201810286398 A CN201810286398 A CN 201810286398A CN 108508065 A CN108508065 A CN 108508065A
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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
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The present invention relates to a kind of gas sensitives and preparation method thereof for detecting trace concentration toluene, belong to gas sensitive technical field.The gas sensitive arranged by nickel ferrite based magnetic loaded spiral skeleton nano wire cubic periodic, has the connection of 25 nanometers of length between skeleton nano wire, and two kinds of different size of mesoporous distributions are differently formed according to distance between nano wire；A diameter of 5 8.5 nanometers of skeleton nano wire；177 216m of specific surface area2/g。
Description
Technical field
The present invention relates to a kind of gas sensitives and preparation method thereof for detecting trace concentration toluene, belong to gas sensitive
Technical field.
Background technology
It is well known that toluene is a kind of important Organic Chemicals, while being also largely used as solvent and high-octane rating vapour
Oil additive is widely used in the industries such as oil, resin and plastic, rubber, leather, but toluene gas is inflammable, volatile, to skin
Skin, mucous membrane are irritant, and Central nervous system has anesthetic effect, have serious harm to environment, therefore the World Health Organization advises
It is within 70ppb to determine toluene concentration limit value in room air.In addition, the toluene in characteristics of contaminated respiratory droplets gas is the important of detection lung cancer
Potential source biomolecule marker (toluene concentration in healthy human body exhaled gas usually in 20-30ppb, and patients with lung cancer exhaled gas
Middle toluene concentration then significantly rises to 80-100ppb).Therefore it is special to effective detection of (especially trace concentration) toluene gas
Important.
The detection method of toluene gas mainly has gas phase or liquid chromatography, spectrophotometer method, quartz crystal micro- at present
Measure scale method, Fiber Optical Sensor Based circle etc., but these methods still have some shortcomings, as equipment it is expensive, it is complicated for operation, detect when
Between it is long, cannot scene in real time detection etc..Toluene semiconductor gas sensor refers to that will partly be led to the sensitive metal oxide of toluene
The gas sensor that body is prepared into plus electrode and adding thermal resistance, it has simple in structure, high sensitivity, performance stabilization, cost
It is low, be easy to miniaturization and the features such as portability, toluene can be measured in real time, be had great application prospect.As it
The toluene gas sensitive generally use of middle key component be the metals such as cobalt, tin, tungsten oxide or composite oxides.Such as Liu
Et al. use mesoporous Co3O4It is 22.55 to 100ppm toluene sensitivity as sensitive material, Monitoring lower-cut is 1ppm (S
Liu,ZY Wang,HR Zhao,T Fei,T Zhang.Ordered mesoporous Co3O4for high-performance
toluene sensing.Sensors and Actuators B-Chemical,2014,197(3):342-349)；Qiao etc.
People uses the SnO of loading Pd2Nanocages are 2.7 to 1ppm toluene sensitivity as sensitive material, Monitoring lower-cut 100ppb
(L Qiao,YF Bing,YZ Wang,SS Yu,ZZ Liang,Y Zeng.Enhanced toluene sensing
performances of Pd-loaded SnO2cubic nanocages with porous nanoparticle-
assembled shells.Sensors and Actuators B-Chemical,2017,241:1121-1129)；Tian etc.
People uses the flower-shaped SnO of loading Pd2Microballoon is 0.58 to 80ppb toluene sensitivity as sensitive material, and Monitoring lower-cut is
80ppb(JL Tian,J Wang,YW Hao,HY Du,XG Li.Toluene sensing properties of porous
Pd-loaded flower-like SnO2microspheres.Sensors and Actuators B-Chemical,2014,
202:795-802)；Shan et al. uses SnO2-Fe2O3Composite nano tube is sensitive material, when operating temperature is 260 DEG C
24.3 is reached to 50ppm toluene sensitivity, Monitoring lower-cut be 50ppb (H Shan, CB Liu, L Liu, JB Zhang, HY Li,
Z Liu,XB Zhang,XQ Bo,X Chi.Excellent Toluene Sensing Properties of SnO2-
Fe2O3Interconnected Nanotubes.ACS Applied Materials&Interfaces,2013,5(13):
6376-6380).But high sensitivity, stability are good, toluene gas sensitive of the Monitoring lower-cut less than 2ppb still needs further
Exploitation.
Invention content
It is an object of the invention to overcome the defect of the above-mentioned prior art, provide that a kind of high sensitivity, stability is good, detection
Lower limit is less than a kind of ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton and preparation method thereof of 2ppb.
The ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton is arranged by nickel ferrite based magnetic loaded spiral skeleton nano wire cubic periodic
It arranges, has the connection of 2-5 nanometers of length between skeleton nano wire, two kinds of differences are differently formed according to distance between nano wire
The mesoporous distribution of size；A diameter of 5-8.5 nanometers of skeleton nano wire；Specific surface area 177-216m2/g。
Preparation method comprises the following steps：
A), surfactant, water and strong acid, preferably concentrated hydrochloric acid mix at 35-100 DEG C, stir 1-12 hours until surface is lived
Property agent all dissolve and be uniformly dispersed, be then added n-butanol, after stirring 2 hours, ethyl orthosilicate TEOS, stirring 24 be added
After hour, be transferred to a polytetrafluoroethylene (PTFE) (in bottle, then 40 DEG C of hydro-thermal reactions 1 day, through suction filtration, washing, room temperature after natural cooling
It spontaneously dries, i.e. the mesopore silicon oxide containing surfactant；
B) mesopore silicon oxide without surfactant is obtained after, being removed within 6 hours by 550 DEG C in air calcinings；
C) it is, 1 by molar ratio:Heating is fused into liquid after 2 nickel nitrate is mixed with ferric nitrate, and it is processed that step b is then added
Mesopore silicon oxide, 70 DEG C repeatedly grinding uniformly after be heated in air 750-900 DEG C calcine 2-10 hour, calcining heat up
Rate is 0.5-2.5 DEG C/min；
D) it is, 1 by molar ratio:Heating is fused into liquid after 2 nickel nitrate is mixed with ferric nitrate, and sample obtained by step c is then added
Product are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air, and calcining heating rate is 1 DEG C/min；
E) 2-10M strong base solutions, preferably NaOH solution, are added into the product after calcining, centrifugal filtration is to remove Jie after stirring
Hole silica template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton.
The ratio between pore volume of the volume of nitrate and mesopore silicon oxide is 0.5-0.8 in the step c and d:1, the body of nitrate
The ratio between product and pore volume of mesopore silicon oxide too it is small cannot obtain orderly mesoporous nickel ferrite based magnetic loaded, too it is big then can only obtain it is single mesoporous
Mesoporous nickel ferrite based magnetic loaded.
The present invention has following effect：
1) material it is unique, with two different mesoporous diffusions being distributed with conducive to gas molecule, accelerate response resume speed：
The order mesoporous nickel ferrite based magnetic loaded of ultra-fine skeleton provided by the invention is arranged by nickel ferrite based magnetic loaded spiral skeleton nano wire cubic periodic, bone
Has the connection of 2-5 nanometers of length between frame nano wire, two kinds of mesoporous distribution proportions can be by adjusting mesopore silicon oxide template
Aperture and the ratio between the pore volume of volume and mesopore silicon oxide of connectivity and nitrate control, the sky between skeleton nano wire
Gap is conducive to the diffusion of gas molecule, accelerates response resume speed；
2) sensitivity is enhanced：Material specific surface area 177-216m provided by the invention2/ g, large specific surface area, material surface are lived
Property bit number of points it is more, enhancing material and gas interacts, and then enhances the sensitivity to toluene gas；
3) thermal stability is enhanced：It is 2-5nm connections to have length between skeleton nano wire in material provided by the invention, is subtracted
The mutual contact of skeleton nano wire is lacked, can reduce under the sensitivity that sintering phenomenon and specific surface area loss are brought under high temperature
Drop, enhances thermal stability；
4) its air-sensitive property can be changed：The diameter of skeleton nano wire in material provided by the invention can be mesoporous by adjusting
The aperture of silica template controls, and can change its air-sensitive property accordingly.
5) the excessively high gained mesopore silicon oxide of hydrothermal temperature cannot prepare double mesoporous knots with it for template in the step a
Structure.
Description of the drawings
Fig. 1：For the pore size distribution collection of illustrative plates of the 1 ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton of gained of embodiment；
Fig. 2：For the TEM pictures of the 1 ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton of gained of embodiment；
Fig. 3：It is air-sensitive response curve of the ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton of the gained of embodiment 1 to various concentration toluene gas.
Fig. 4, it is air-sensitive response curve of the ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton of the gained of embodiment 6 to various concentration toluene gas.
Specific implementation mode
Embodiment 1
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Then, it is removed within 6 hours by 550 degree in air calcinings
A white powder is obtained after going.The ordered meso-porous silicon oxide specific surface area 736m of gained2/ g, pore volume 0.64cm3/ g, pore size is about
For 4.8nm.
After 0.0016 molar nitric acid nickel is mixed with 0.0032 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.56g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；Heating is fused into liquid after 0.0015 molar nitric acid nickel is mixed with 0.003 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in body, being heated to 750 DEG C in air after 70 DEG C repeatedly grinding uniformly calcines 6 hours,
Calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove Jie after stirring
Hole silica template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton, material specific surface area 216m2/ g,
Pore volume 0.39cm3/g。
Such as the pore size distribution collection of illustrative plates that Fig. 1 is the ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton obtained by the present embodiment, show it with 2 kinds not
With the mesoporous distribution of size；Such as the TEM pictures that Fig. 2 is the ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton obtained by the present embodiment, it was demonstrated that it has
Orderly meso-hole structure；As at a temperature of Fig. 3, which works for the ultra-fine order mesoporous nickel ferrite based magnetic loaded of skeleton obtained by the present embodiment at 230 DEG C, to be known
Air-sensitive response to various concentration toluene gas reaches 77.3 to 1ppm toluene gas susceptibilitys, and Monitoring lower-cut is (quick less than 2ppb
0.44) sensitivity reaches, and common ferrous acid nickel particles only have 1 to the susceptibility of 1ppm toluene gas, shows its significant enhancing
Effect.
Embodiment 2
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Then, it is removed within 6 hours by 550 degree in air calcinings
A white powder is obtained after going.The ordered meso-porous silicon oxide specific surface area 736m of gained2/ g, pore volume 0.64cm3/ g, pore size is about
For 4.8nm.
After 0.0015 molar nitric acid nickel is mixed with 0.003 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.56g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；Heating is fused into liquid after 0.0014 molar nitric acid nickel is mixed with 0.028 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in body, being heated to 750 DEG C in air after 70 DEG C repeatedly grinding uniformly calcines 6 hours,
Calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove Jie after stirring
Hole silica template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton.
Embodiment 3
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Sample surfaces activating agent P123 passes through in sky obtained by front
550 degree of calcinings obtain a white powder after removing within 6 hours in gas.The ordered meso-porous silicon oxide specific surface area 736m of gained2/ g, hole body
Product 0.64cm3/ g, pore size are about 4.8nm.
After 0.001 molar nitric acid nickel is mixed with 0.002 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.56g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；It heats and is fused into after 0.0009 molar nitric acid nickel is mixed with 0.0018 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in liquid, it is small to be heated to 750 DEG C of calcinings 6 in air after 70 DEG C repeatedly grinding uniformly
When, calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove after stirring
Mesopore silicon oxide template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton.
Embodiment 4
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Sample surfaces activating agent P123 passes through in sky obtained by front
550 degree of calcinings obtain a white powder after removing within 6 hours in gas.The ordered meso-porous silicon oxide specific surface area 736m of gained2/ g, hole body
Product 0.64cm3/ g, pore size are about 4.8nm.
After 0.0014 molar nitric acid nickel is mixed with 0.0028 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.56g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；It heats and is fused into after 0.0013 molar nitric acid nickel is mixed with 0.0026 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in liquid, it is small to be heated to 750 DEG C of calcinings 6 in air after 70 DEG C repeatedly grinding uniformly
When, calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove after stirring
Mesopore silicon oxide template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton.
Embodiment 5
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Sample surfaces activating agent P123 passes through in sky obtained by front
550 degree of calcinings obtain a white powder after removing within 6 hours in gas.The ordered meso-porous silicon oxide specific surface area 736m of gained2/ g, hole body
Product 0.64cm3/ g, pore size are about 4.8nm.
After 0.0013 molar nitric acid nickel is mixed with 0.0026 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.56g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；It heats and is fused into after 0.0012 molar nitric acid nickel is mixed with 0.0024 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in liquid, it is small to be heated to 750 DEG C of calcinings 6 in air after 70 DEG C repeatedly grinding uniformly
When, calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove after stirring
Mesopore silicon oxide template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton.
Embodiment 6
6.0g surfactants P123,216g water is mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stirs 12 hours until surface-active
Agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicate TEOS are added,
It after stirring 24 hours, is transferred in a polytetrafluoroethylene (PTFE) bottle, then 100 degree of hydro-thermal reactions 1 day, through filtering, washing after natural cooling
It washs, natural drying at room temperature, i.e. the mesopore silicon oxide containing surfactant.Sample surfaces activating agent P123 passes through in sky obtained by front
550 degree of calcinings obtain a white powder after removing within 6 hours in gas.The ordered meso-porous silicon oxide specific surface area 877m of gained2/ g, hole body
Product 1cm3/ g, pore size are about 7.9nm.
After 0.0016 molar nitric acid nickel is mixed with 0.0032 molar nitric acid iron heating be fused into liquid, be then added with
The above-mentioned processed mesopore silicon oxides of 1.12g are heated to 750 DEG C after grinding is uniform repeatedly at 70 DEG C and calcine 6 hours in air,
Calcining heating rate is 1 DEG C/min；Heating is fused into liquid after 0.0015 molar nitric acid nickel is mixed with 0.003 molar nitric acid iron again
Then sample obtained by above-mentioned steps is added in body, being heated to 750 DEG C in air after 70 DEG C repeatedly grinding uniformly calcines 6 hours,
Calcining heating rate is 1 DEG C/min；2M NaOH solutions are added into the product after calcining, centrifugal filtration is to remove Jie after stirring
Hole silica template to get to the present invention the order mesoporous ferrous acid nickel material of ultra-fine skeleton, material specific surface area 177m2/ g,
Pore volume 0.39cm3/ g reaches 44.24 to 1ppm toluene gas susceptibilitys, and less than 2ppb, (susceptibility reaches Monitoring lower-cut
0.1)。
Claims (6)
1. a kind of order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of ultra-fine skeleton, it is characterized in that：The material toluene gas sensitive is
It is arranged by nickel ferrite based magnetic loaded spiral skeleton nano wire cubic periodic.
2. a kind of ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton as described in claim 1, it is characterized in that：The material
Expect the connection for having 2-5 nanometers of length between middle skeleton nano wire, according between nano wire distance to be differently formed two kinds of differences big
Small mesoporous distribution；A diameter of 5-8.5 nanometers of skeleton nano wire；Specific surface area 177-216m2/g。
3. a kind of ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton as described in claim 1, it is characterized in that：It is prepared
Method includes the following steps：
A), 6.0g surfactants P123,216g water are mixed with 11.8g concentrated hydrochloric acids at 35 DEG C, stir 1-12 hours until table
Face activating agent is all dissolved and is uniformly dispersed, and 6g n-butanols are then added, and after stirring 2 hours, 12.9g ethyl orthosilicates are added
TEOS is transferred in a polytetrafluoroethylene (PTFE) bottle, then 40 DEG C of hydro-thermal reactions 1 day, after stirring 24 hours through taking out after natural cooling
Filter, washing, natural drying at room temperature, the i.e. mesopore silicon oxide containing surfactant；
B), sample surfaces activating agent P123 obtained by front is obtained after being removed within 6 hours by 550 DEG C in air calcinings and is lived without surface
The mesopore silicon oxide of property agent；
C) after, 0.0016 molar nitric acid nickel is mixed with 0.0032 molar nitric acid iron heating be fused into liquid, be then added with
The processed mesopore silicon oxides of 1.56g steps b are hard template, and 750 DEG C are heated in air after 70 DEG C repeatedly grinding uniformly
Calcining 6 hours, calcining heating rate are 1 DEG C/min；
D) heating is fused into liquid after, mixing 0.0015 molar nitric acid nickel with 0.003 molar nitric acid iron, and step c is then added
Gained sample, 70 DEG C repeatedly grinding uniformly after be heated in air 750 DEG C calcine 6 hours, calcining heating rate be 1 DEG C/
min；
E) 2M NaOH solutions, are added into the product after calcining, centrifugal filtration is to remove mesopore silicon oxide template after stirring, i.e.,
Obtain the order mesoporous ferrous acid nickel material of ultra-fine skeleton of the present invention.
4. a kind of preparation method of the ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton as claimed in claim 3, special
Sign is：35-100 DEG C of hydrothermal temperature in the step a.
5. a kind of ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton as claimed in claim 3, it is characterized in that：The step
The ratio between the pore volume of the volume of nitrate and mesopore silicon oxide is 0.5-0.8 in rapid c and d:1, the volume of nitrate and mesoporous oxygen
The ratio between pore volume of SiClx is too small cannot to be obtained orderly mesoporous nickel ferrite based magnetic loaded, then can only obtain very much single mesoporous mesoporous ferrous acid greatly
The molar ratio of nickel, ferric nitrate and nickel nitrate is 2:1, calcination temperature is 750-900 DEG C, and heating rate is 0.5-2.5 DEG C/min, is forged
The burning time is 2-10h.
6. a kind of ultra-fine order mesoporous nickel ferrite based magnetic loaded toluene gas sensitive of skeleton as claimed in claim 3, it is characterized in that：The step
A concentration of 2-10M of sodium hydroxide solution in rapid e.
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| CN110665506A (en) * | 2019-09-18 | 2020-01-10 | 宁夏大学 | Tetracycline photocatalytic degradation material and preparation method thereof |
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| XIAOHONG SUN 等: "Enhanced Gas-Sening Performance of Fe-Doped Ordered Mesoporous NiO with Long-Range Periodicity", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| XIAOYONG LAI: "Ordered mesoporous NiFe2O4 with ultrathin framework for low-ppb toluene sensing", 《SCIENCE BULLETIN》 * |
| 赖小勇: "几种介孔材料的硬模板法制备及其气敏性质研究", 《中国博士学位论文全文数据库工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109772334A (en) * | 2018-12-28 | 2019-05-21 | 宁夏大学 | A kind of big mesoporous nickel cobalt glucose-sensitive material of high-specific surface area and preparation method thereof |
| CN110665506A (en) * | 2019-09-18 | 2020-01-10 | 宁夏大学 | Tetracycline photocatalytic degradation material and preparation method thereof |
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