CN110451579A - A kind of dispersion Fe2O3Preparation method - Google Patents
A kind of dispersion Fe2O3Preparation method Download PDFInfo
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- 239000006185 dispersion Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title description 4
- 238000003756 stirring Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- 239000000047 product Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960001484 edetic acid Drugs 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002086 nanomaterial Substances 0.000 claims abstract description 9
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 8
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 6
- 230000002045 lasting effect Effects 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims description 5
- 230000035945 sensitivity Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 33
- 239000000463 material Substances 0.000 description 22
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 18
- 239000002245 particle Substances 0.000 description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- 239000000523 sample Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 229910000859 α-Fe Inorganic materials 0.000 description 8
- 239000002585 base Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010218 electron microscopic analysis Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000006101 laboratory sample Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
Classifications
-
- 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
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of dispersion Fe2O3Preparation method weighs Fe (NO3)3·9H2O, which is dissolved in deionized water, obtains solution A；Deionized water is added under stirring into solution A, persistently stirs to obtain solution B；Ethylenediamine tetra-acetic acid is added in solution B, it is lasting to stir, obtain solution C；Sodium acetate trihydrate is weighed, deionized water is added under stirring and continues to stir to obtain solution D；Solution D is quickly adding into solution C under stirring, it is lasting to stir, obtain solution E；E solution is imported in ptfe autoclave liner, capping kettle is placed in baking oven and reacts；Reaction kettle is taken out, is placed at room temperature, product is poured out after cooling down completely, is washed repeatedly with deionized water, finally use ethanol washing, simultaneously drying is sampled, obtains target product；Target product is obtained into final product ferric oxide nano-material after Muffle furnace high-temperature calcination half an hour.The beneficial effects of the invention are as follows preparation methods to be simple and efficient, and pollen can not only play the role of improving dispersibility, mould pattern, can also enhance sensitivity, improve the effects of selectivity.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of α-Fe2O3The preparation method of nano material.
Background technique
The seventies and eighties in last century, iron oxide gas sensing property material are developed, other semiconductor materials such as ZnO and SnO2Deng
Gas sensing property material mostly requires although having developed fairly perfect by a certain amount of noble metal ability of doping
Their sensitivity is set to increase.However iron oxide gas sensing property material is but in contrast, in addition common metal ion
In the case of can have preferable gas-sensitive property, and such gas sensing property material has excellent adhesion, institute on base material
It is more convenient to make gas sensor.Iron oxide gas sensing property material with ZnO, SnO2Together, become three big gas sensing properties
Material.Wherein, α-Fe2O3It is in iron oxide gas sensing property material for making the most important one kind of gas sensor.The material is in lithium
The application study of ion battery, gas sensor, magnetic material, pigment, catalyst etc. is significantly.And have
There are special size and shape that can cause the change of respective performances, exactly because this characteristic makes the research to the material big
It is big to increase.At the same time, the rapid development of modern industry, people are rapid to the pay attention to day by day of domestic environment and new industry
The application range and potential value of gas sensor have further been widened in emergence etc..Therefore, to α-Fe2O3Nano material gas
The further investigation and improvement of quick performance are significantly.But it is many kinds of in face of under test gas, use environment is complicated more
The problems such as change, the sensitivity of the material and selectivity can't fully meet actual demand, need to continue to improve preparation method and come
Further increase the air-sensitive performance of material.
Nowadays, people are growing to good days demand.But with the development of the times, industrial production develops more
Add rapidly.More and more poisonous gas, imflammable gas and explosion hazard gas can be generated, environment is polluted, influences the strong of people
Health life.Metal oxide semiconductor gas sensor can be used as monitor and detection instrument, being capable of sensitive, accurately and effectively monitoring inspection
These harmful imflammable gas are surveyed, wherein α-Fe2O3Gas sensing property material has good gas sensing property and stability, can be than calibrated
Really forecast and detect pernicious gas.Therefore, the detection monitoring device prepared using the material development is very promising.
Summary of the invention
The purpose of the present invention is to provide a kind of dispersion Fe2O3Preparation method, the beneficial effects of the invention are as follows preparation method letters
It is single efficient, and pollen can not only play the role of improving dispersibility, mould pattern, can also enhance sensitivity, improve choosing
The effects of selecting property.
The technical scheme adopted by the invention is that following the steps below:
1. weighing Fe (NO3)3·9H2O, which is dissolved in deionized water, obtains solution A；
2. deionized water is added under stirring into solution A, solution B is persistently stirred to obtain；
3. a small spoon EDTA ethylenediamine tetra-acetic acid is added in solution B under stirring, it is lasting to stir, obtain solution C；
4. weighing sodium acetate trihydrate, deionized water is added under stirring and continuing to stir to obtain solution D；
5. solution D is quickly adding into solution C under stirring, it is lasting to stir, obtain solution E；
6. E solution is imported in ptfe autoclave liner, capping kettle is placed in baking oven and reacts；
7. taking out reaction kettle, it is placed at room temperature, product is poured out after cooling down completely, is washed repeatedly with deionized water, most
Ethanol washing is used afterwards, is sampled and dry, is obtained target product；
8. target product is obtained final product ferric oxide nano-material after Muffle furnace high-temperature calcination half an hour.
Further,
1 weighs Fe (NO3)3·9H2O2.0200g is dissolved in 20mL deionized water and obtains solution A；
2. 30mL deionized water is added under stirring into solution A, persistently stirs 5min and obtain solution B；
3. a small spoon EDTA ethylenediamine tetra-acetic acid is added in solution B under stirring, 10min is persistently stirred, is obtained
Solution C；
20mL deionized water is added 4. weigh sodium acetate trihydrate 4.0824g, under stirring and continues to stir 5min and obtains
Solution D；
5. solution D is quickly adding into solution C under stirring, 10min is persistently stirred, obtains solution E；
6. E solution is imported in 100mL ptfe autoclave liner, capping kettle is placed in baking oven at 120 DEG C
React 6h；
7. taking out reaction kettle, it is placed at least 6h at room temperature, product is poured out after cooling down completely, is washed repeatedly with deionized water
It washs 10 times, finally uses ethanol washing 2-3 times, sample and dry, obtain target product；
8. obtaining final product di-iron trioxide nanometer material after target product to be calcined to half an hour at 500 DEG C of Muffle furnace
Material.
Detailed description of the invention
Fig. 1 is Fe2O3(N) X ray diffracting spectrum；
Fig. 2 is Fe2O3(N) and Fe2O3(P) transmission electron microscope picture；
Fig. 3 is Fe2O3(P) at different temperatures to the sensitivity histogram of 100ppm isopropanol.
Specific embodiment
The present invention is described in detail With reference to embodiment.
The present invention disperses Fe2O3Steps are as follows for preparation method:
1. weighing Fe (NO3)3·9H2O2.0200g is dissolved in 20mL deionized water and obtains solution A；
2. 30mL deionized water is added under stirring into solution A, persistently stirs 5min and obtain solution B；
3. a small spoon EDTA ethylenediamine tetra-acetic acid is added in solution B under stirring, 10min is persistently stirred, is obtained
Solution C；
20mL deionized water is added 4. weigh sodium acetate trihydrate 4.0824g, under stirring and continues to stir 5min and obtains
Solution D；
5. solution D is quickly adding into solution C under stirring, 10min is persistently stirred, obtains solution E；
6. E solution is imported in 100mL ptfe autoclave liner, capping kettle is placed in baking oven at 120 DEG C
React 6h；
7. taking out reaction kettle, it is placed at least 6h at room temperature, product is poured out after cooling down completely, is washed repeatedly with deionized water
It washs 10 times, finally uses ethanol washing 2-3 times, sample and dry, obtain target product；
8. repeating the above steps, sodium acetate trihydrate aqueous solution in step 4 is added 0.5000g pollen and (steeps in advance
20min) compare experiment；
9. obtaining final product di-iron trioxide nanometer material after target product to be calcined to half an hour at 500 DEG C of Muffle furnace
Material；
10. sample number into spectrum, the sample number into spectrum to addition pollen preparation is α-Fe2O3(P) no the sample of addition pollen preparation is not compiled
Number be α-Fe2O3(N)。
X-ray diffraction analysis
To determine whether the prepared powder of this experiment is α-Fe2O3Nano material carries out X-ray diffraction to laboratory sample
Analysis.By the diffraction maximum and α-Fe of Fig. 1 derived sample2O3Standard diagram (JCPDSNo.79-1741) it is completely the same, without it
He occurs miscellaneous peak.Spreading out at 24.1 °, 33.2 °, 35.7 °, 41.0 °, 49.7 °, 54.0 °, 57.6 °, 62.3 ° and 63.90 °
It penetrates peak and corresponds respectively to α-Fe2O3(012), (104), (110), (113), (024), (116), (018), (214) of standard diagram
(300) crystal face.Therefore, the material of this experiment synthesis is pure phase α-Fe2O3Nano material, and each characteristic peak is more sharp, says
It is bright that there is good crystallinity.It can then predict that the reaction occurred in the hydro-thermal reaction stage is Fe3++3OH-→Fe(OH)3, forging
Burning the reaction that the stage of reaction occurs is 2Fe (OH)3→Fe2O3+3H2O。
Transmitted electron electron-microscopic analysis
To analyze α-Fe2O3Microscopic appearance, granular size and particle diameter distribution have carried out transmitted electron electricity to laboratory sample
Sub- microscopic analysis.Take a small amount of sample in the dehydrated alcohol of 5mL, ultrasonic disperse for a period of time, takes a small amount of solution drop in Electronic Speculum
Copper mesh on, using the particle size of transmission electron microscope observation sample, pattern and dispersion.
As shown in Fig. 2, (a) is with ethylenediamine tetra-acetic acid (EDTA) for surfactant in Fig. 2, water is the α-of solvent preparation
Fe2O3(N) transmission plot of nano-powder, as we can see from the figure without apparent boundary, nearly all adhesion between particle and particle
Together, reunite than more serious.(b) is it can be seen that powder is in elliposoidal substantially in Fig. 2, it can be seen that individual particle, particle size
About 60nm.(c) is the α-Fe prepared after the identical lower addition pollen of other experiment conditions in Fig. 22O3(P) nano-powder is saturating
Figure is penetrated, it can be found that α-Fe after pollen is added2O3The pattern of nano-powder has changed a lot, and dispersion effect has significantly
Progress, (d) is presented irregular it can be seen that the pattern that nano particle after pollen is added has occurred biggish variation in Fig. 2
Square crystal particle, particle size is about 100nm.It can be seen that agglomeration weakens, nano particle microscopic appearance after addition pollen
It is all changed with granular size.
α-Fe2O3The research of air-sensitive performance
An important indicator for measuring gas sensor performance is the optimum working temperature of gas sensor, in lower work temperature
Degree has lower power consumption.To determine α-Fe2O3The optimum working temperature of base gas sensor, experiment test α-Fe2O3(P) In
To the response of 100ppm isopropanol gas at 110~370 DEG C.
As shown in fig. 3, it was found that α-the Fe when temperature range is 110~260 DEG C2O3(P) base gas sensor is to 100ppm isopropyl
The sensitivity of alcohol gradually rises, and the α-Fe when temperature range is 260~370 DEG C2O3(P) base gas sensor is to 100ppm isopropyl
The sensitivity of alcohol gradually weakens.That is α-the Fe at 260 DEG C2O3(P) base gas sensor is to the sensitivity highest of 100ppm isopropanol,
About 12 or so.Thus may determine that the optimum working temperature of the gas sensor is 260 DEG C.
The present invention using nine water ferric nitrates as source of iron, sodium acetate trihydrate is alkali source, deionized water is solvent, ethylenediamine tetrem
Sour (EDTA) is surfactant.Whether to add pollen as unitary variant, α-Fe is prepared under 120 DEG C of hydro-thermal reaction2O3It receives
Rice flour end.
It is found by X-ray diffraction analysis (XRD), the diffraction maximum and α-Fe of sample2O3Standard diagram (JCPDSNo.79-
1741) completely the same, occur without other miscellaneous peaks and each characteristic peak is more sharp.The material for illustrating this experiment synthesis is pure phase
α-Fe2O3Nano material, and there is good crystallinity.
It is found by transmitted electron electron-microscopic analysis (TEM), α-Fe2O3(N) without apparent boundary between nano particle
Limit, is nearly all sticked together, and reunites than more serious.And α-Fe2O3(P) dispersion effect of nano particle has significant progress,
Biggish variation has occurred in granule-morphology.Illustrate that the effect that pattern improves dispersibility of moulding can be played by adding pollen.
It is found by air-sensitive performance test analysis, the α-Fe under the isopropanol gas of 100ppm2O3(P) base gas sensor
Optimum working temperature is 260 DEG C, at this temperature to the sensitivity highest of 100ppm isopropanol, about 12.It is in operating temperature
α-Fe at 260 DEG C2O3(P) sensitivity and selectivity are all than α-Fe2O3(N) height.
Therefore, being added into pollen not only can play the role of improving dispersibility, mould pattern, can also enhance sensitive
Degree improves the effects of selectivity.The addition of pollen inhibits product to reunite at least in terms of following two: 1 hydro-thermal reaction stage, flower
The presence of powder particles can provide carrier for the load of iron oxide, while its irregular movement can stir solution and Fe (OH) 3
Grain prevents particle bonding from reuniting.2 use Muffle furnace heat treatment stages: heat treatment stages be reunite be easiest to the spot stage it
One.The presence of pollen is first is that isolation Fe (OH) 3, is separated from each other the Fe2O3 generated in its decomposable process and after decomposing, the group of reduction
It is poly- to occur；CO2 gas is generated second is that decomposing under pollen high temperature, gas overflowing can also promote particle dispersion, inhibit to reunite.Pollen
Addition increases product α-Fe2O3Dispersibility, and then promote its air-sensitive performance.
The above is only not to make limit in any form to the present invention to better embodiment of the invention
System, any simple modification that embodiment of above is made according to the technical essence of the invention, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (2)
1. a kind of dispersion Fe2O3Preparation method, it is characterised in that follow the steps below:
1. weighing Fe (NO3)3·9H2O, which is dissolved in deionized water, obtains solution A；
2. deionized water is added under stirring into solution A, solution B is persistently stirred to obtain；
3. a small spoon EDTA ethylenediamine tetra-acetic acid is added in solution B under stirring, it is lasting to stir, obtain solution C；
4. weighing sodium acetate trihydrate, deionized water is added under stirring and continuing to stir to obtain solution D；
5. solution D is quickly adding into solution C under stirring, it is lasting to stir, obtain solution E；
6. E solution is imported in ptfe autoclave liner, capping kettle is placed in baking oven and reacts；
7. taking out reaction kettle, it is placed at room temperature, product is poured out after cooling down completely, is washed with deionized water, is finally used repeatedly
Ethanol washing samples and dry, obtains target product；
8. target product is obtained final product ferric oxide nano-material after Muffle furnace high-temperature calcination half an hour.
2. according to a kind of dispersion Fe described in claim 12O3Preparation method, it is characterised in that:
1. described 1 weighs Fe (NO3)3·9H2O2.0200g is dissolved in 20mL deionized water and obtains solution A；
2. 30mL deionized water is added under stirring into solution A, persistently stirs 5min and obtain solution B；
3. a small spoon EDTA ethylenediamine tetra-acetic acid is added in solution B under stirring, 10min is persistently stirred, solution is obtained
C；
20mL deionized water is added 4. weigh sodium acetate trihydrate 4.0824g, under stirring and continues to stir 5min and obtains solution
D；
5. solution D is quickly adding into solution C under stirring, 10min is persistently stirred, obtains solution E；
6. E solution is imported in 100mL ptfe autoclave liner, capping kettle is placed in baking oven and reacts at 120 DEG C
6h；
7. taking out reaction kettle, it is placed at least 6h at room temperature, product is poured out after cooling down completely, washs 10 repeatedly with deionized water
It is secondary, it finally uses ethanol washing 2-3 times, samples and dry, obtain target product；
8. obtaining final product ferric oxide nano-material after target product to be calcined to half an hour at 500 DEG C of Muffle furnace.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910770443.1A CN110451579A (en) | 2019-08-20 | 2019-08-20 | A kind of dispersion Fe2O3Preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910770443.1A CN110451579A (en) | 2019-08-20 | 2019-08-20 | A kind of dispersion Fe2O3Preparation method |
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| Publication Number | Publication Date |
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| CN110451579A true CN110451579A (en) | 2019-11-15 |
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| CN114314677A (en) * | 2022-01-12 | 2022-04-12 | 宁波大学 | Nano hydrated iron oxide and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049977A (en) * | 2007-05-15 | 2007-10-10 | 河北师范大学 | Method for preparing Nano Fe2O3 |
| CN103101972A (en) * | 2012-12-04 | 2013-05-15 | 西安交通大学 | Preparation method of three-dimensional mesoporous titanium dioxide photocatalyst by means of biological template method |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN109179511A (en) * | 2018-08-02 | 2019-01-11 | 济南大学 | A kind of ferric oxide nano ball material with triethylamine sensitlzing effect |
-
2019
- 2019-08-20 CN CN201910770443.1A patent/CN110451579A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049977A (en) * | 2007-05-15 | 2007-10-10 | 河北师范大学 | Method for preparing Nano Fe2O3 |
| CN103101972A (en) * | 2012-12-04 | 2013-05-15 | 西安交通大学 | Preparation method of three-dimensional mesoporous titanium dioxide photocatalyst by means of biological template method |
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN109179511A (en) * | 2018-08-02 | 2019-01-11 | 济南大学 | A kind of ferric oxide nano ball material with triethylamine sensitlzing effect |
Non-Patent Citations (4)
| Title |
|---|
| 孔超: "利用松花粉模板制备 MgAl-LDHs/MgFe2O4 及其吸附性能的研究", 《中国优秀硕士学位论文数据库》 * |
| 曹煜: "以花粉为模板合成不同结构多孔氧化铈材料", 《苏州科技学院学报（工程技术版）》 * |
| 李平: "以油菜花粉为模板水热法制备TiO2中空微球", 《无机材料学报》 * |
| 路禄: "氧化铁基磁性微球的制备及其吸附性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314677A (en) * | 2022-01-12 | 2022-04-12 | 宁波大学 | Nano hydrated iron oxide and preparation method and application thereof |
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Application publication date: 20191115 |