CN109368706A - A kind of classifying porous α-Fe of three-dimensional of Pd modification2O3Material and the preparation method and application thereof - Google Patents
A kind of classifying porous α-Fe of three-dimensional of Pd modification2O3Material and the preparation method and application thereof Download PDFInfo
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- CN109368706A CN109368706A CN201810991589.4A CN201810991589A CN109368706A CN 109368706 A CN109368706 A CN 109368706A CN 201810991589 A CN201810991589 A CN 201810991589A CN 109368706 A CN109368706 A CN 109368706A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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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 invention discloses a kind of classifying porous α-Fe of three-dimensional of Pd modification2O3Material and preparation method thereof, and application of the material in detection ethylene gas is provided.The present invention greatly improves α-Fe by the catalytic action of noble metal nano particles Pd2O3Material reduces detection limit to the detection sensitivity of ethylene gas, realizes that the high sensitivity to ethylene gas, low detection limits detect.Three-dimensional classifying porous α-Fe2O3Structure not only provides more adsorption sites for absorption Pd nano particle, while big specific surface area is also beneficial to adsorb more ethylene gas.So Pd nano particle and three-dimensional classifying porous α-Fe2O3Synergistic effect realize to the detection of the high sensitivity and low detection limits of ethylene gas.
Description
Technical field
The present invention relates to a kind of three-dimensional porous α-Fe of Pd modification2O3Structural material and its preparation method and application belongs to new
Material Field.
Background technique
Ethylene gas judges fruit maturity as a Plant Hormone, by the ethylene gas of detection fruit release
Grade has very important significance for fruit picking, processing and storage.Ethylene is flammable explosive gas simultaneously, mixed with air
Conjunction can form explosive mixture, if meeting open fire, high fever or contacting with oxidant, there is the danger for causing combustion explosion.And it is logical
The ethylene contents crossed in detection characteristics of contaminated respiratory droplets gas can also be used in the lipid peroxidation for analyzing human inner cell, and then analyze
The lesion of intracorporeal organ studies the pathogenesis of related disease, achievees the purpose that effectively to prevent by early detection.Therefore efficiently
Rapidly detection ethylene gas is crucial industry, agricultural and biological health.
The detection difficulty of ethylene gas is high, and sensitivity is low, and is mostly high temperature detection.The method of traditional detection ethylene is main
It is red, orange, green, blue, yellow (ROGBY), time and effort consuming, using flexible is poor.Sensor technology, optical detective technology and detection technique of fluorescence etc.
Though also having been reported that for ethylene detection, it is often detected, and limit is not high, and sensitivity is poor, it is difficult to realize to the fast of low-concentration ethane
Fast high sensitivity detection.Therefore, development to the fast high-sensitive detection technique and method of low-concentration ethane be it is very necessary and
Significant.
Metal oxide semiconductor nano-material is since its unique advantage is widely used in air-sensitive research, such as α-Fe2O3
The n-type semiconductor for being 2.1eV as a kind of band gap width is commonly used to detection liquefied petroleum gas, alcohol gas, acetone gas, sulphur
Change hydrogen, but its sensitivity is low, and there are problems that cross sensitivity.
Summary of the invention
The purpose of the present invention is to provide a kind of classifying porous α-Fe of three-dimensional of Pd modification2O3Material and preparation method thereof, and
Application of the material in detection ethylene gas is provided.
A kind of classifying porous α-Fe of three-dimensional of Pd modification of the invention2O3Material, wherein α-Fe2O3Structure is by flake
α-Fe2O3Flower-shaped α-Fe made of self assembly stacks2O3, Pd is nano-particle modified in α-Fe2O3Lamella on, Pd nano particle
Size is distributed between 10-30nm.
A kind of classifying porous α-Fe of three-dimensional of Pd modification of the present invention2O3The preparation method of material, including amorphous state contain
The preparation step of iron predecessor, the preparation step of Pd nano particle, by Pd nano particle be adsorbed onto step on predecessor and
Calcining step.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that the amorphous state
The preparation step of iron content predecessor includes:
(1) by FeCl3·6H2O, urea, tetrabutylammonium bromide are dissolved in ethylene glycol, and dissolution is sufficiently stirred, is heated to 170-
200 DEG C, to the complete greening of solution colour；
(2) it by the centrifugation of above-mentioned product, washing, dries to get amorphous state iron content predecessor is arrived.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that Pd nanometers described
The preparation step of particle includes:
(1) it takes palladium chloride to be dissolved in hydrochloric acid, polyvinylpyrrolidone is taken to be dissolved in ethylene glycol, two kinds of solution are slowly added to simultaneously
Into 100-150 DEG C of ethylene glycol；
(2) after above-mentioned solution reaction 10-20min, NaOH solution is taken to be added, persistently stirs 8- at 100-150 DEG C
10h obtains the solution of the nano particle containing Pd.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that described to receive Pd
The step that rice grain is adsorbed on amorphous state iron content predecessor is to take the preparation step of Pd nano particle obtained containing Pd nanometers
Iron content predecessor is added in the solution of particle, in 40-60 DEG C of shaking table reaction of temperature, makes Pd nano particle uniform adsorption in predecessor
Lamella on.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that the calcining step
It suddenly is to calcine 1-3h at 300-400 DEG C.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that including following steps
It is rapid:
Step 1: by 0.5-0.8g FeCl3·6H2O, 1.2-1.5g urea, 3-4g tetrabutylammonium bromide are dissolved in 80-100mL
In ethylene glycol, dissolution is sufficiently stirred, is heated to 170-200 DEG C, to the complete greening of solution colour；
Step 2: the centrifugation of above-mentioned product, washing are dried to get amorphous state iron content predecessor is arrived；
Step 3: taking 0.07-0.09g palladium chloride to be dissolved in the 0.15-0.2g/mL hydrochloric acid of 2ml, take 0.08-0.1g polyethylene pyrrole
Pyrrolidone is dissolved in 4-6mL ethylene glycol, and two kinds of solution are slowly added in 100-150 DEG C of ethylene glycol simultaneously；
Step 4: after above-mentioned solution reaction 10-20min, the NaOH solution of 6-7mL 0.006-0.007g/mL is taken to be added,
8-10h is persistently stirred at 100-150 DEG C, obtains the solution of the nano particle containing Pd；
Step 5: taking predecessor powder obtained in step 2, the solution containing Pd nano particle is added, by it in temperature
40-60 DEG C of shaking table reacts 4-6 hours, makes Pd nano particle uniform adsorption on the lamella of amorphous state predecessor；Shaking speed is
200~300rmp；
Step 6: the amorphous state predecessor for being adsorbed with Pd nano particle being calcined into 1-3h at 300-400 DEG C to get Pd is arrived
Classifying porous α-the Fe of three-dimensional of modification2O3Structure.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that the step 2
In, revolving speed when centrifugal treating is 5000~7000r/min, and carrying out washing treatment is alternately to be washed 3-5 times respectively with water and ethyl alcohol；It is dry
Temperature is 50-70 DEG C, drying time 10-13h.
Classifying porous α-the Fe of three-dimensional of Pd modification described above2O3In the preparation method of material, it is preferred that the step 6
In, heating rate is 1~3 DEG C/min, when cooling, is down to room temperature with furnace.
Classifying porous α-the Fe of three-dimensional of Pd modification of the present invention2O3Material can be applied to the detection of ethylene gas.It is detecting
It, can be by the classifying porous α-Fe of three-dimensional of Pd modification in2O3Material is coated to the ceramic tube table of common gas detection sensor
Face.The present invention realizes the structure to the high sensitivity of ethylene gas using the catalytic action that Pd is broken ethylene gas carbon-carbon double bond
Detection.Specific embodiment are as follows: take appropriate above-mentioned material to be dispersed in ethanol solution, take the Pd of 5~10 μ L to modify with liquid-transfering gun
The classifying porous α-Fe of three-dimensional2O3The suspension of material, is applied on the ceramic tube of sensor, coats material uniformly to ceramic tube
Surface.Then the sensor for applying good material is put into gas chamber, is heated to 300 DEG C, aging 2-5h, by certain density ethylene gas
Body is passed through gas chamber, after reacting 2-4min, is passed through air, drives ethylene gas out of gas chamber, by being passed through gas front and back material resistance
The ratio of variation realizes the detection to gas sensitivity, and specific test result is as shown in Fig. 4.
The present invention is conducive to the absorption and expansion of gas by the flower-shaped three-dimensional hierarchical structure that porous ultrathin nanometer piece is self-assembled into
It dissipates, meanwhile, noble metal nano particles are modified to the surface of this hierarchical structure by electrostatic interaction, your gold can be efficiently used
The catalytic action of metal nano-particle.The present invention has constructed one kind by α-Fe2O3The three-dimensional that porous nano-sheet is self-assembled into is classifying porous
Structure, while the nano particle for going up Pd is modified in its lamellar structure, its response sensitivity is improved using the synergistic effect of the two.
The invention has the benefit that by the catalytic action of noble metal nano particles Pd, (catalytic action of Pd is conducive to
Ethylene gas carbon-carbon double bond it is broken), α-Fe can be greatly improved2O3Material reduces the detection sensitivity of ethylene gas simultaneously
Detection limit realizes that the high sensitivity to ethylene gas, low detection limits detect, and makes the three-dimensional porous α-Fe of Pd modification of the present invention2O3Material
Expect the gas sensitive preferably as ethylene gas detection.Three-dimensional classifying porous α-Fe2O3Structure is not only absorption Pd nano particle
More adsorption sites are provided, while big specific surface area is also beneficial to adsorb more ethylene gas.So Pd nano particle
With three-dimensional porous classification α-Fe2O3Synergistic effect realize to the detection of the high sensitivity and low detection limits of ethylene gas.Simultaneously originally
Invention discovery, when the adsorbance (using EDS spectroscopy detection) of Pd is 2%~3.5%, the catalytic action of Pd is most strong, right
The ethylene gas of 1000ppm, detection sensitivity are 46 or so, and test temperature is 300 DEG C, specific detection performance such as attached drawing 4 and attached
Shown in Fig. 5.
Detailed description of the invention
Fig. 1 is the three-dimensional porous α-Fe of this Pd modification2O3The flow chart of materials synthesis passes through simple hydro-thermal method first
Predecessor is made, is then adsorbed in Pd nano particle on the lamella of this three-dimensional hierarchical structure, finally by calcining, predecessor
Phase transition occurs, the α-Fe of crystalline state is converted by amorphous state2O3, simultaneously because calcination process has gas generation, in α-
Fe2O3Lamella on generate a large amount of hole, ultimately form Pd modification three-dimensional porous α-Fe2O3Structure.
Fig. 2 is the SEM figure of products therefrom in material synthesis processes of the present invention, and (a) figure is the predecessor that hydro-thermal method obtains
SEM figure, it can be clearly seen that it is this stacked as thin slice made of flower-like structure；(b) figure is obtained after calcining predecessor
Three-dimensional classifying porous α-Fe2O3SEM figure, clearly visible this flower-shaped α-Fe in figure2O3It is produced on the lamella of structure a large amount of
Hole；(c) figure is in the classifying porous α-Fe of this three-dimensional2O3SEM figure after having modified Pd nano particle on the lamella of structure.
The XRD spectra that Fig. 3 is.It can be seen from the figure that initially the predecessor as made from hydro-thermal method is a kind of amorphous state
(amorphous) structure has then obtained the good α-Fe of crystalline state by calcining2O3, when the modification amount of Pd is less, in XRD spectra
There is no the peaks corresponding to Pd, but when the content of the Pd of modification reaches 4.65%, the peak of Pd can be clearly visible in XRD spectra,
As shown in Figure 2.
Fig. 4 be embodiment products therefrom is placed in it is measured quick in the ethylene gas atmosphere that concentration is 100~1500ppm
Feel performance diagram, operating temperature is 300 DEG C.As seen from the figure embodiment products therefrom to the response speed of ethylene quickly,
It is restorative good, and have to the ethylene of 1000ppm up to 46 response sensitivity, response sensitivity is reaction front and back material resistance
Ratio.When the concentration of ethylene gas reaches 1500ppm, response tends to be saturated.
Fig. 5 is the three-dimensional classification α-Fe of different Pd modification amounts at 300 DEG C of optimum working temperature2O3Structure is to 500ppm second
The response sensitivity line chart of alkene gas.As seen from the figure, as this three-dimensional classification α-Fe2O3Structural modification Pd nano particle with
Afterwards, the response sensitivity of ethylene gas is greatly improved, and its sensitivity highest when the modification amount of Pd is 2~3.5%.It inserts
It is, to the response curve of the ethylene gas of 1ppm, as seen from the figure, to work as ethylene gas when the modification amount of Pd is 2~3.5% in figure
When the concentration of body is 1ppm, still there is response, response is 2 or so.It can be seen that the three-dimensional of 2~3.5%Pd modification amount point
Grade α-Fe2O3Structure is to the minimum detectability of ethylene gas up to 1ppm.
Specific embodiment
Embodiment
Classifying porous α-the Fe of three-dimensional of Pd modification of the present invention2O3Material preparation method is as follows:
Step 1: by 0.6g FeCl3·6H2O, 1.35g urea, 3.6g tetrabutylammonium bromide are dissolved in 90mL ethylene glycol, fill
Divide stirring and dissolving, 170 DEG C is heated to, to the complete greening of solution colour.
Step 2: the centrifugation of above-mentioned product, washing are dried to get flower-shaped amorphous iron content predecessor powder is arrived.
Step 3: taking 0.085g palladium chloride to be dissolved in the hydrochloric acid of 2ml, 0.2g/mL, 0.08g polyvinylpyrrolidone is taken to be dissolved in
Two kinds of solution are slowly added in 120 DEG C of ethylene glycol by 5mL ethylene glycol simultaneously.
Step 4: after above-mentioned solution reaction 15min, taking the NaOH solution of 6.5mL, 0.007g/mL to be added, at 120 DEG C
9h is persistently stirred, the solution of the nano particle containing Pd is obtained.
Step 5: taking predecessor powder obtained in a certain amount of step 2, be separately added into different amounts of nano particle containing Pd
Solution, by its in temperature 50 C shaking table react 5h, shaking speed 250rpm, make Pd nano particle uniform adsorption before flower-shaped
On the lamella for driving object.
Step 6: the flower-shaped predecessor for being adsorbed with different content Pd nano particle is calcined into 2h at 350 DEG C to get to not
With the classifying porous α-Fe of three-dimensional of Pd modification amount2O3Structure.
Application examples
By the classifying porous α-Fe of three-dimensional of the Pd modification of embodiment preparation2O3Material is dispersed in ethanol solution, with shifting
Classifying porous α-the Fe of three-dimensional that liquid rifle takes 5~10 μ LPd to modify2O3The suspension of material is coated to the ceramic pipe surface of sensor,
Coat material uniformly to the surface of ceramic tube.The sensor for being coated with sensitive material is placed in gas chamber, test temperature is heated to
300 DEG C, 2~5h of aging is passed through ethylene gas and is detected, and after reacting 2~4min, is passed through air, ethylene gas is driven out of,
The response sensitivity to ethylene gas is indicated by the ratio of material resistance value before and after ethylene adsorption gas.Test result shows
Classifying porous α-the Fe of three-dimensional of 2~3.5% Pd modification2O3Material is to the detection sensitivity highest of ethylene gas, at 300 DEG C
Under operating temperature to the response sensitivity of the ethylene gas of 1000ppm be 46 or so and minimum detectability up to 1ppm.
Claims (8)
1. a kind of classifying porous α-Fe of three-dimensional of Pd modification2O3Material, wherein α-Fe2O3Structure is by laminar α-Fe2O3From
Flower-shaped α-Fe made of assembling stacks2O3, Pd is nano-particle modified in α-Fe2O3Lamella on, Pd nanoparticle size is distributed in
Between 10-30nm.
2. a kind of classifying porous α-Fe of three-dimensional of Pd modification2O3The preparation method of material, the preparation including amorphous state iron content predecessor
Step, the preparation step of Pd nano particle, the step and calcining step Pd nano particle being adsorbed on predecessor.
3. the classifying porous α-Fe of three-dimensional of Pd modification as claimed in claim 22O3The preparation method of material, which is characterized in that described
The preparation step of amorphous state iron content predecessor includes:
(1) by FeCl3·6H2O, urea, tetrabutylammonium bromide are dissolved in ethylene glycol, and dissolution is sufficiently stirred, is heated to 170-200
DEG C, to the complete greening of solution colour；
(2) it by the centrifugation of above-mentioned product, washing, dries to get amorphous state iron content predecessor is arrived.
4. the classifying porous α-Fe of three-dimensional of Pd modification as claimed in claim 22O3The preparation method of material, which is characterized in that described
The preparation step of Pd nano particle includes:
(1) it takes palladium chloride to be dissolved in hydrochloric acid, polyvinylpyrrolidone is taken to be dissolved in ethylene glycol, two kinds of solution are slowly added into simultaneously
In 100-150 DEG C of ethylene glycol；
(2) after above-mentioned solution reaction 10-20min, NaOH solution is taken to be added, 8-10h is persistently stirred at 100-150 DEG C, i.e.,
The solution of the nano particle containing Pd is made.
5. the classifying porous α-Fe of three-dimensional of Pd modification as claimed in claim 22O3The preparation method of material, which is characterized in that described
It is to take the preparation step of Pd nano particle is obtained to contain by the step that Pd nano particle is adsorbed on amorphous state iron content predecessor
Iron content predecessor is added in the solution of Pd nano particle, in 40-60 DEG C of shaking table reaction of temperature, Pd nano particle uniform adsorption is made to exist
On the lamella of predecessor.
6. the classifying porous α-Fe of three-dimensional of Pd modification as claimed in claim 22O3The preparation method of material, which is characterized in that described
Calcining step is to calcine 1-3h at 300-400 DEG C.
7. the classifying porous α-Fe of three-dimensional that the Pd as described in claim any one of 2-6 is modified2O3The preparation method of material, feature
It is, includes the following steps:
Step 1: by 0.5-0.8g FeCl3·6H2O, 1.2-1.5g urea, 3-4g tetrabutylammonium bromide are dissolved in 80-100mL second two
In alcohol, dissolution is sufficiently stirred, is heated to 170-200 DEG C, to the complete greening of solution colour；
Step 2: the centrifugation of above-mentioned product, washing are dried to get amorphous state iron content predecessor is arrived；
Step 3: taking 0.07-0.09g palladium chloride to be dissolved in the 0.15-0.2g/mL hydrochloric acid of 2ml, take 0.08-0.1g polyvinylpyrrolidine
Ketone is dissolved in 4-6mL ethylene glycol, and two kinds of solution are slowly added in 100-150 DEG C of ethylene glycol simultaneously；
Step 4: after above-mentioned solution reaction 10-20min, the NaOH solution of 6-7mL 0.006-0.007g/mL is taken to be added,
8-10h is persistently stirred at 100-150 DEG C, obtains the solution of the nano particle containing Pd；
Step 5: taking predecessor powder obtained in step 2, the solution containing Pd nano particle is added, by it in temperature 40-60
DEG C shaking table reacts 4-6 hours, makes Pd nano particle uniform adsorption on the lamella of amorphous state iron content predecessor；Shaking speed is
200~300rmp；
Step 6: the predecessor for being adsorbed with Pd nano particle is calcined into 1-3h at 300-400 DEG C to get the three-dimensional modified to Pd
Classifying porous α-Fe2O3Structure.
8. the classifying porous α-Fe of three-dimensional of the modification of Pd described in claim 12O3Material or as described in claim any one of 2-7
Classifying porous α-the Fe of three-dimensional for the Pd modification that preparation method obtains2O3Application of the material in ethylene gas detection.
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