CN107720831B - Ferric oxide nano-material and its application based on solvent-thermal method controlledly synthesis - Google Patents
Ferric oxide nano-material and its application based on solvent-thermal method controlledly synthesis Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 title abstract description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title description 2
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 20
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 16
- 239000004065 semiconductor Substances 0.000 abstract description 11
- 239000002904 solvent Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000004044 response Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 239000003446 ligand Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 3
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 abstract description 2
- FFRUQSUMDFNBLG-UHFFFAOYSA-N 2-(2,4,5-trichlorophenoxy)ethyl 2,2,2-trichloroacetate Chemical compound ClC1=CC(Cl)=C(OCCOC(=O)C(Cl)(Cl)Cl)C=C1Cl FFRUQSUMDFNBLG-UHFFFAOYSA-N 0.000 abstract 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 4
- 239000004312 hexamethylene tetramine Substances 0.000 description 4
- 229960004011 methenamine Drugs 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- 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]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G01—MEASURING; TESTING
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Abstract
The invention discloses a kind of α-Fe based on solvent-thermal method controlledly synthesis2O3Nano material and its application are to achieve the purpose that controlledly synthesis multi-level nano-structure by changing solvent chain length and adjusting solvent polarity, belong to nano-functional material preparation field.It is specifically with FeCl3For reaction source substance, hexa or sodium carbonate are ligand, obtain α-Fe first by solvent-thermal method2O3Then it is calcined in air atmosphere and obtains the α-Fe of multilevel structure by precursor2O3Nanometer powder.In gained α-Fe2O3After terpinol grinding is added in nanometer powder, uniformly it is applied to be placed in Muffle furnace on ceramic tube and is sintered, can be prepared by α-Fe2O3Multilevel structure gas sensor.The gas sensor has the characteristic that response is fast, stability is high, selectivity is high, can be used for preparing semiconductor gas sensor.
Description
Technical field
The invention belongs to nano-functional material preparation technical fields, and in particular to a kind of based on solvent-thermal method controlledly synthesis
α-Fe2O3Nano material and its application that gas sensor is prepared as gas sensor.
Background technique
Currently, air quality problems are still the huge challenge that many countries face.One comfortable clean air
Environment is the important guarantee that people improve the quality of living, it is therefore necessary to be detected to air quality.Gas is detected
Common approach have electrochemical process, solid electrolyte method, infrared absorption method, chemoluminescence method, surface acoustic wave sensor, gas phase color
Spectrum and gas sensor etc..In these methods, gas sensor method is considered as the method for ideal detection air.One side
Face has the advantages that easy to operate, high sensitivity, fast response time, recovery time are short；On the other hand, such sensor is easy
In control surface microenvironment, by changing the nanostructure and composition of oxide gas sensor, so that effective influence senses
The sensing capabilities of device.
A kind of device of the gas sensor as detection gas, basic functional principle are gas molecule and semiconductor nano
O occurs between material2Adsorption/desorption and the interactions such as redox reaction influence the electric conductivity of material, thus will be by
The concentration or component for surveying gas are converted to corresponding electric signal, according to the strong and weak concentration for analyzing tested gas of the electric signal of acquisition
Etc. relevant informations, and then play detection, monitoring and the forewarning function to pernicious gas.At this stage, gas sensor mainly towards
The directions such as low energy consumption, multi-functional, low concentration detection, high sensitivity are developed.
Semiconductor gas sensor is as a member in gas sensor large family, mainly with transition metal oxide half
Conductor material is as gas sensitive.The sensitivity characteristic of transition metal oxide semiconductor material decides the good of sensor performance
It is bad.However, the sensitivity of Metal Oxide Gas Sensors is affected by various factors, such as 1. density and mobility of carrier；
2. the Surface Modification Effect；3. quantum size effect；4. the chemical property of specific surface area size and material surface.The first two factor can
Regulated and controled by sensing material type (free electron in N-shaped and p-type semiconductor) and doped chemical type；Latter two factors by
The pattern of material, shape and size control.Therefore, the element the Nomenclature Composition and Structure of Complexes pattern of semiconductor is special to the sensitivity of semiconductor material
Property has an important influence.And compared to the synthetic methods such as presoma thermal decomposition method, sol-gal process, template, solvent-thermal method side
Method have preparation process is simple, easy to operate, crystallization degree is good, can effectively realize the controlledly synthesis of nanometer material structure and pattern
The advantages that.
In transition metal oxide, α-Fe2O3It is a kind of typical n-type semiconductor, because it is with good optical band gap
The advantages that (eV of Eg=2.1), high corrosion-resistant, natural abundance and nontoxicity and low cost, is widely used in optical electro-chemistry, sensing
The fields such as device.But traditional α-Fe2O3Semiconductor sensitive material there is sensitivity low, poor selectivity, response recovery time
The disadvantages of long.Meanwhile α-the Fe of special level structure2O3Semiconductor usually has different from its construction unit and block materials
Unique physico-chemical property.In recent years, a large amount of α-Fe2O3For example porous club shaped structure of level material, hollow ball structure, flower-like structure
Application of the equal gas-sensitive nano materials on gas sensor, make its sensitivity, selectivity and in terms of
To biggish improvement.Therefore, it is based on solvent thermal process, designs novel reaction system control synthesis α-Fe2O3Multilevel structure air-sensitive
Element has realistic meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of α-Fe based on solvent-thermal method controlledly synthesis2O3Nano material and its application,
It is to realize controlledly synthesis α-Fe by changing solvent chain length and adjusting solvent polarity2O3Purpose, and then prepare a series of
Practicability semi-conductor type gas sensor highly sensitive, response is fast, stability is good, at low cost.
To achieve the above object, the present invention adopts the following technical scheme:
One kind being based on solvent-thermal method controlledly synthesis α-Fe2O3The method of multilevel structure gas sensor comprising following steps:
(1) it takes anhydrous ferric trichloride and ligand to be put into beaker, reaction dissolvent, the temperature constant magnetic stirring at 50 DEG C is added
1h；
(2) mixture obtained by step (1) is put into autoclave, is placed in 220 DEG C of baking ovens and reacts 6h；
(3) step (2) products therefrom is placed in Muffle furnace, in 500 DEG C of air atmospheres after centrifugation, washing, drying
3h is calcined, the α-Fe of multilevel structure is obtained2O3Nanometer powder.
The molar ratio of anhydrous ferric trichloride and ligand is 1:1 ~ 1:2 in step (1)；Wherein, the ligand is hexa-methylene
Tetramine (HMTA) or sodium carbonate.
Reaction dissolvent described in step (1) is ethylene glycol, methanol or ethyl alcohol.
α-the Fe2O3Nano material can be used as gas sensitive, be further used for the system of gas sensor in gas sensor
It is standby；Its gas sensor the preparation method comprises the following steps: weighing α-Fe described in 5-10 mg2O3It is equal that 1 drop terpinol grinding is added in nano material
It is even, then it is uniformly applied on ceramic tube, naturally dry is placed in Muffle furnace, is sintered 2h at 300 DEG C to get α-
Fe2O3Multilevel structure gas sensor.
The beneficial effects of the present invention are:
(1) on the basis of solvent-thermal method, by changing solvent chain length and adjusting solvent polarity, controlledly synthesis goes out the present invention
A series of α-the Fe of different structures2O3Nano material, resulting materials have structure uniformly, that preparation is simple, thermal stability is good etc. is excellent
Gesture.
(2) in terms of air-sensitive performance test, resulting materials of the present invention show the excellent selectivity to acetone, and low
There is biggish sensitivity under concentration, while also improving α-Fe2O3When material restores the sensitivity and response of reducibility gas
Between.
(3) provided by the invention to be based on solvent-thermal method controlledly synthesis α-Fe2O3The method of structure can have specific for synthesis
The Nano-function thin films of structure and excellent air-sensitive performance are offered reference.
Detailed description of the invention
Fig. 1 is α-Fe prepared by embodiment one2O3The XRD diagram of precursor product.
Fig. 2 is α-Fe prepared by one~embodiment of embodiment five2O3The XRD diagram of nanometer powder.
Fig. 3 is α-Fe prepared by one~embodiment of embodiment five2O3The SEM of nanometer powder schemes.
Fig. 4 is with one~embodiment of embodiment, five gained α-Fe2O3The air-sensitive performance of the gas sensor of nanometer powder preparation is surveyed
Attempt.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment one,
(1) the anhydrous FeCl of 0.152g is weighed3With 0.140g HMTA in clean beaker, the stirring of 40mL ethylene glycol is added
Dissolution is placed in 50 DEG C of constant temperature stirring 1h on magnetic stirring apparatus；
(2) above-mentioned solution is put into autoclave, is placed in 220 DEG C of baking ovens and reacts 6h；
(3) to product cooled to room temperature, precipitating is collected by centrifugation, is repeatedly washed with deionized water and dehydrated alcohol, then
It is placed in air and spontaneously dries, obtain α-Fe2O3Precursor；α-the Fe that will be obtained2O3Precursor salt is placed in Muffle furnace, 500
3h is calcined in DEG C air atmosphere, obtains the α-Fe of multilevel structure2O3Nanometer powder is labeled as S1；
Fig. 1 is α-Fe prepared by embodiment one2O3The XRD diagram of precursor product.It can be seen from figure 1 that the precursor substance is
A kind of ferrite compound.
Embodiment two,
The additional amount for implementing HMTA in one is changed to 0.280 g, remaining operation is as in the first embodiment, obtain the α-of multilevel structure
Fe2O3Nanometer powder is labeled as S2.
Embodiment three,
The reaction dissolvent for implementing to be added in one is changed to methanol, remaining operation is as in the first embodiment, obtain multilevel structure
α-Fe2O3Nanometer powder is labeled as S3.
Example IV,
The reaction dissolvent for implementing to be added in one is changed to ethyl alcohol, remaining operation is as in the first embodiment, obtain multilevel structure
α-Fe2O3Nanometer powder is labeled as S4.
Embodiment five,
The HTMA for implementing to be added in one is replaced with to the Na of 0.106g2CO3, remaining operation is as in the first embodiment, obtain multistage knot
α-the Fe of structure2O3Nanometer powder is labeled as S5.
Fig. 2 is α-Fe prepared by one~embodiment of embodiment five2O3The XRD diagram of nanometer powder.It can be seen that all
The diffraction maximum of sample can belong to the α-Fe of rhombohedral system structure well2O3(JCPDS33-0664), and without any miscellaneous
Peak shows that product is pure α-Fe2O3。
Fig. 3 is α-Fe prepared by one~embodiment of embodiment five2O3The SEM of nanometer powder schemes.It can be seen that S1 is
Band-like porous structure α-Fe2O3, nanometer tape thickness is in 50-100nm, and for width in 400-700nm, length is longer, is distributed in 1-3 μm；
S2 is three-dimensional flower-shaped structure α-Fe2O3, average-size 650nm is about 40nm by thickness, and the wide nanometer sheet in 300-400nm is logical
Central point interconnection is crossed to be composed；S3 is class hollow ball structure α-Fe2O3, size is smaller, about 100nm, and particle diameter distribution
It is more uniform；α-Fe obtained by S42O3It is the diamond structure of about 300nm, surface is rougher, can be clearly seen that the product by small
Nanoparticle aggregate forms；S5 is thin banded structure, with a thickness of between 30-60nm, width within the scope of 200nm-350nm,
And porous structure is more obvious.
Application examples,
Weigh the α-Fe of gained multilevel structure in 5-10 mg embodiment one ~ five2O3Nanometer powder is separately added into 1 drop pine tar
It uniformly, is then uniformly applied on ceramic tube, naturally dry is placed in Muffle furnace, is sintered at 300 DEG C by alcohol grinding
2h obtains corresponding gas sensor Q1-Q5.
The air-sensitive performance that Fig. 4 is gained gas sensor Q1-Q5 is tested, wherein figure (a) is sample to various concentration acetone gas
The sensitivity curve figure of body, figure (b) are response-recovery curve of the sample to 100ppm alcohol gas.By scheming (a) as it can be seen that acetone
For concentration before 500ppm, gas sensor sensitivity increasing degree is larger, continues growing the change of acetone concentration sensitivity increasing degree
Small, illustrating sensor at low concentrations has biggish sensitivity；By scheming (b) as it can be seen that prepared α-Fe2O3Gas sensor exists
By still having preferable response after several circulations, show that the stability of gas sensitive is preferable.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (1)
1. a kind of α-Fe based on solvent-thermal method controlledly synthesis2O3Nano material, it is characterised in that: the following steps are included:
(1) the anhydrous FeCl of 0.152g is weighed3With 0.106g Na2CO3In clean beaker, it is molten that the stirring of 40mL ethylene glycol is added
Solution is placed in 50 DEG C of constant temperature stirring 1h on magnetic stirring apparatus；
(2) above-mentioned solution is put into autoclave, is placed in 220 DEG C of baking ovens and reacts 6h；
(3) to product cooled to room temperature, precipitating is collected by centrifugation, is repeatedly washed with deionized water and dehydrated alcohol, then be placed in
It is spontaneously dried in air, obtains α-Fe2O3Precursor；α-the Fe that will be obtained2O3Precursor salt is placed in Muffle furnace, at 500 DEG C
3h is calcined in air atmosphere, obtains the α-Fe of multilevel structure2O3Nanometer powder.
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| CN109987640B (en) * | 2019-04-29 | 2020-07-31 | 北京科技大学 | Preparation of nano α -Fe2O3Method (2) |
| CN111250120A (en) * | 2020-02-21 | 2020-06-09 | 上海应用技术大学 | Phosphotungstic acid modified nano iron oxide SCR denitration catalyst and preparation method and application thereof |
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