CN112897593B - Regular polyhedral alpha-Fe 2 O 3 Method for preparing self-growing material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 60
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 13
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 claims abstract description 10
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 claims abstract description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229940079101 sodium sulfide Drugs 0.000 claims description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- ZGHLCBJZQLNUAZ-UHFFFAOYSA-N sodium sulfide nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[S-2] ZGHLCBJZQLNUAZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 44
- 239000000919 ceramic Substances 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 229910018487 Ni—Cr Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 4
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 229940116411 terpineol Drugs 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- -1 SnO 2 Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
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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]
-
- 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
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- 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
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- 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
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a regular polyhedral alpha-Fe 2 O 3 The preparation method and application of the self-growing material are characterized in that firstly, trivalent ferric salt, urea and sodium dodecyl sulfate are subjected to hydrothermal reaction to obtain a FeOOH precursor; then FeOOH and sodium sulfide nonahydrate are further hydrothermally treated to obtain regular polyhedral alpha-Fe 2 O 3 Self-growing the material. The method has the advantages of simple operation, low cost and controllable synthesis process, and the prepared material has good crystallinity and regular and controllable appearance. The regular polyhedral alpha-Fe prepared by the invention 2 O 3 The self-growing material has important application prospect in the field of gas sensors.
Description
Technical Field
The invention belongs to the technical field of gas sensors. In particular to a regular polyhedral alpha-Fe 2 O 3 A preparation method and application of the self-growing material.
Background
Due to human activity, ammonia and various volatile organic compounds are released in large quantities into the atmosphere, bringing about a certain degree of environmental risk. In order to accurately detect different types of polluted gases, a large number of gas-sensitive sensor materials with high reliability and convenient use are developed and developed. The gas sensor plays an important role in the aspects of chemical industry, environmental protection, public safety, human health and the like. Metal oxides, e.g. SnO 2 、ZnO、Fe 2 O 3 And V 2 O 5 When exposed to an oxidizing or reducing gas, the material changes its electrical resistance, and thus functions as a gas-sensitive material. The resistance change of the semiconductor oxide material is closely related to the shape of the material, the ambient temperature and the type and concentration of ambient gas, and has great development prospect in the field of gas sensing. However, commercial sensors of semiconducting metal oxides still suffer from drawbacks that limit their widespread use, such as limited maximum sensitivity, work efficiencyHigh working temperature and lack of long-term stability.
α- Fe 2 O 3 Is one of the n-type semiconductor materials, the most stable iron oxide under ambient conditions (Eg = 2.1 eV). The photocatalyst has the characteristics of low cost, high photocatalytic activity, good electrochemical performance, environmental protection and the like, and is widely used as a catalyst, a gas sensor material and an electrode material. So far, people mainly prepare alpha-Fe with various morphologies by a hydrothermal method, a sol-gel method, a pulse discharge method, a coprecipitation method and the like 2 O 3 The material and the physical and chemical properties thereof are studied. Better regulate and control alpha-Fe 2 O 3 The micro-morphology of the material and the improvement of the gas-sensitive performance of the material, and how to optimize the experimental conditions become a research hotspot in the field of gas sensors. Therefore, a simple and efficient method is designed to prepare the alpha-Fe with good crystallinity, regular morphology and controllability 2 O 3 The material has important research significance in the field of gas sensors.
Disclosure of Invention
The invention aims to provide a gas-sensitive material alpha-Fe applied to a gas sensor 2 O 3 The synthesis method has the advantages of simple and convenient operation, low cost and controllable synthesis process, and the prepared material has good crystallinity and regular and controllable appearance.
In order to achieve the purpose, the invention adopts the following technical scheme.
Regular polyhedral alpha-Fe 2 O 3 The preparation method of the self-growing material comprises the following steps:
1) Adding trivalent ferric salt, urea and sodium dodecyl sulfate into deionized water, and stirring to obtain a transparent solution;
2) Carrying out hydrothermal reaction on the transparent solution obtained in the step 1), and carrying out suction filtration, washing and drying on a product to obtain a FeOOH precursor;
3) Adding the FeOOH precursor prepared in the step 2) and sodium sulfide nonahydrate into deionized water, and stirring to obtain a uniform solution;
4) Carrying out hydrothermal reaction on the uniform solution obtained in the step 3), and then carrying out reaction on the obtained productFiltering, washing and drying to obtain regular polyhedral alpha-Fe 2 O 3 Self-growing the material.
In the step 1), the molar ratio of the trivalent ferric salt to the urea to the sodium dodecyl sulfate is 1.
In the step 1), the concentration of the ferric salt in the deionized water is 0.5 mol/L; the ferric salt is preferably an iron halide.
In the step 2), the hydrothermal reaction temperature is 90 ℃, and the reaction time is 20 h; the hydrothermal reaction is carried out under sealed conditions.
In the step 2), washing is carried out for 6 to 10 times by using deionized water and ethanol.
In the step 2), the drying conditions are as follows: drying for 10 to 20 hours at 60 to 80 ℃ in a common way.
In the step 3), the molar ratio of the FeOOH precursor to the sodium sulfide nonahydrate is 1 to 6-30.
In the step 3), the concentration of the sodium sulfide in the deionized water is 0.1 to 0.5 mol/L.
In the step 4), the hydrothermal reaction temperature is 180 to 200 ℃, and the reaction time is 12 to 24 hours; the hydrothermal reaction is carried out under sealed conditions.
In the step 4), the washing times are 6 to 10 times by using deionized water and ethanol.
In the step 4), the drying conditions are as follows: drying at 60-80 ℃ for 15-20 h.
Regular polyhedral alpha-Fe 2 O 3 The self-growing material is applied to a gas sensor and is specifically implemented as follows:
the prepared material and terpineol are fully mixed to form uniform slurry, the slurry is coated on a ceramic tube (a pair of gold electrodes are arranged on the ceramic tube and connected together by four platinum wires), and a Ni-Cr resistance wire serving as a heater penetrates through the ceramic tube to be connected into a gas sensor measuring system for gas-sensitive characteristic test.
The invention has the following advantages:
the invention provides regular polyhedral alpha-Fe 2 O 3 The synthesis method of the self-growing material comprises the preparation before and after the hydrothermal methodPreparing FeOOH precursor and alpha-Fe 2 O 3 Two steps. The method has the advantages of good controllability of the hydrothermal reaction process, simple and convenient operation, mild reaction conditions, high safety, novel appearance of the obtained product, high stability and the like. The invention obtains the regular polyhedral self-growing structure formed by FeOOH as a precursor by reasonably adjusting the proportion and concentration of ferric salt, sodium dodecyl sulfate and sodium sulfide nonahydrate, the hydrothermal reaction temperature, time and the like. In the hydrothermal reaction process, deionized water is used as a solvent, ferric salt is used as an iron source, sodium dodecyl sulfate is used as a surfactant, and sodium sulfide nonahydrate is used as a stabilizer, so that the materials are easily obtained, and the reaction conditions are simple. Wherein, the surfactant sodium dodecyl sulfate is used for preparing the alpha-Fe 2 O 3 In the process, crystallization can be inhibited, micron particles can be prevented from agglomerating, and the particle size can be controlled. The regular polyhedral alpha-Fe prepared by the invention 2 O 3 The self-growing material has important application prospect in the field of gas sensors.
Drawings
FIG. 1 is an XRD pattern of FeOOH precursor synthesized in example 1 of the present invention;
FIG. 2 shows regular polyhedral α -Fe synthesized in example 1 of the present invention 2 O 3 XRD pattern of the self-grown material;
FIG. 3 shows regular polyhedral α -Fe synthesized in example 2 of the present invention 2 O 3 SEM images of self-grown materials;
FIG. 4 shows regular polyhedral α -Fe synthesized in example 3 of the present invention 2 O 3 SEM images of self-grown materials;
FIG. 5 shows regular polyhedral α -Fe synthesized in example 3 of the present invention 2 O 3 The gas sensitive material is used as a relation graph between a sensor signal and gas concentration obtained by testing a gas sensor;
FIG. 6 shows regular polyhedral α -Fe synthesized in example 3 of the present invention 2 O 3 The gas sensitive material is used as a relation graph between a sensor signal obtained by testing a gas sensor and different testing gases.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1 regular polyhedral form of alpha-Fe 2 O 3 Preparation of self-growing materials
1) Adding 35 mmol ferric trichloride hexahydrate (9.460 g), 35 mmol urea (2.102 g) and 2.1 mmol sodium dodecyl sulfate (0.572 g) into 70 mL deionized water, and stirring to obtain a transparent solution;
2) Transferring the solution into a reaction kettle, reacting at 90 ℃ for 20 h, carrying out suction filtration on a product, repeatedly washing with deionized water and ethanol for 6 times to remove impurities, and commonly drying at 80 ℃ for 10 h to obtain a FeOOH precursor;
3) Adding 0.090 g of FeOOH precursor and 2.882 g sodium sulfide nonahydrate into 60 mL deionized water, and stirring to obtain a uniform solution;
4) Transferring the uniform solution into a reaction kettle, reacting at 180 ℃ for 12 h, performing suction filtration on the product, repeatedly washing with deionized water and ethanol for 6 times to remove impurities, and performing common drying at 80 ℃ for 20 h to obtain the regular polyhedral alpha-Fe 2 O 3 Self-growing the material.
Regular polyhedral alpha-Fe 2 O 3 The self-growing material is applied to a gas sensor and is specifically implemented as follows:
the prepared material and terpineol are fully mixed to form uniform slurry, the slurry is coated on a ceramic tube (a pair of gold electrodes are arranged on the ceramic tube and connected together by four platinum wires), and a Ni-Cr resistance wire serving as a heater penetrates through the ceramic tube to be connected into a gas sensor measuring system for gas-sensitive characteristic test.
As shown in FIG. 1, all X-ray diffraction peaks in the figure coincide with those of FeOOH (JCPDS: 34-1266), and the precursor compound is confirmed to be in the FeOOH crystal phase.
As shown in FIG. 2, all X-ray diffraction peaks and α -Fe in the figure 2 O 3 (JCPDS: 33-0664) shows no other impurity phase, indicating that high-purity alpha-Fe is synthesized 2 O 3 The material has excellent crystallinity.
Example 2 regular polyhedral form of alpha-Fe 2 O 3 Preparation of self-growing materials
1) The same as example 1;
2) The same as example 1;
3) Adding 0.090 g of FeOOH precursor and 2.162 g sodium sulfide nonahydrate into 60 mL deionized water, and stirring to obtain a uniform solution;
4) Transferring the uniform solution into a reaction kettle, reacting at 180 ℃ for 12 h, performing suction filtration on the product, repeatedly washing with deionized water and ethanol for 6 times to remove impurities, and performing common drying at 80 ℃ for 20 h to obtain the regular polyhedral alpha-Fe 2 O 3 Self-growing the material.
Regular polyhedral alpha-Fe 2 O 3 The self-growing material is applied to a gas sensor and is specifically implemented as follows:
the prepared material and terpineol are fully mixed to form uniform slurry, the slurry is coated on a ceramic tube (a pair of gold electrodes are arranged on the ceramic tube and connected together by four platinum wires), and a Ni-Cr resistance wire serving as a heater penetrates through the ceramic tube to be connected into a gas sensor measuring system for gas-sensitive characteristic test.
As shown in FIG. 3, high purity alpha-Fe was prepared 2 O 3 The self-growing material is of a micron square structure, and the particle size is less than 3 um.
Example 3 regular polyhedral alpha-Fe 2 O 3 Preparation of self-growing materials
1) The same as example 1;
2) The same as example 1;
3) Adding 0.090 g of FeOOH precursor and 5.764 g sodium sulfide nonahydrate into 60 mL deionized water, and stirring to obtain a uniform solution;
4) Transferring the uniform solution into a reaction kettle, reacting at 180 ℃ for 12 h,filtering the product, repeatedly washing with deionized water and ethanol for 6 times to remove impurities, and drying at 80 deg.C for 20 h to obtain regular polyhedral alpha-Fe 2 O 3 Self-growing the material.
Regular polyhedral alpha-Fe 2 O 3 The self-growing material is applied to a gas sensor and is specifically implemented as follows:
the prepared material and terpineol are fully mixed to form uniform slurry, the slurry is coated on a ceramic tube (a pair of gold electrodes are arranged on the ceramic tube and connected together by four platinum wires), and a Ni-Cr resistance wire serving as a heater penetrates through the ceramic tube to be connected into a gas sensor measuring system for gas-sensitive characteristic test.
As shown in FIG. 4, high purity α -Fe was prepared 2 O 3 The self-growing material is of a micron bipyramid structure, the surface of the material is smooth, the structure is symmetrical, and the particle size is about 10 um.
As shown in fig. 5, from the prepared high purity α -Fe 2 O 3 The sensing signal of the gas sensor assembled as a gas sensitive material to ethanol is far higher than that of other three gases, and at the concentration of 100-900 ppm, the sensing signal of the gas sensor to ethanol, formaldehyde and toluene is enhanced along with the increase of the gas concentration. However, the sensor has a different curve of sensing signal versus gas concentration for methanol, and at concentrations below 700 ppm, the sensing signal increases with increasing gas concentration; when the concentration is higher than 700 ppm, the induced signal decreases as the concentration of the gas increases.
As shown in fig. 6, the gas sensor assembled by using the prepared high-purity α -Fe2O3 as a gas sensitive material has sensing signals of 7.5, 6.6, 5.4 and 2.7 for ethanol, methanol, formaldehyde and toluene, respectively, under the conditions that the test temperature is 370 ℃ and the gas concentration is 500 ppm.
Claims (7)
1. Regular polyhedral alpha-Fe 2 O 3 The preparation method of the self-growing material is characterized by comprising the following steps:
1) Adding trivalent ferric salt, urea and sodium dodecyl sulfate into deionized water, and stirring to obtain a transparent solution;
2) Carrying out hydrothermal reaction on the transparent solution obtained in the step 1), and carrying out suction filtration, washing and drying on a product to obtain a FeOOH precursor;
3) Adding the FeOOH precursor prepared in the step 2) and sodium sulfide nonahydrate into deionized water, and stirring to obtain a uniform solution;
4) Carrying out hydrothermal reaction on the uniform solution obtained in the step 3), carrying out suction filtration, washing and drying on the product to obtain regular polyhedral alpha-Fe 2 O 3 A self-growing material; in the step 1), the molar ratio of the trivalent ferric salt to the urea to the sodium dodecyl sulfate is 1;
in the step 3), the molar ratio of the FeOOH precursor to the sodium sulfide nonahydrate is 1 to 6-30;
in the step 3), the concentration of sodium sulfide in deionized water is 0.1 to 0.5 mol/L; the hydrothermal reaction temperature in the step 4) is 180 to 200 ℃, and the reaction time is 12 to 24 hours; the hydrothermal reaction is carried out under sealed conditions.
2. The regular polyhedral alpha-Fe of claim 1 2 O 3 The preparation method of the self-growing material is characterized in that in the step 1), the concentration of the trivalent ferric salt in the deionized water is 0.5 mol/L; the ferric salt is a halide of iron.
3. The regular polyhedral alpha-Fe of claim 2 2 O 3 The preparation method of the self-growing material is characterized in that in the step 2), the hydrothermal reaction temperature is 90 ℃, and the reaction time is 20 h; the hydrothermal reaction is carried out under sealed conditions.
4. The regular polyhedral alpha-Fe of claim 3 2 O 3 The preparation method of the self-growing material is characterized in that in the step 2), the washing times are 6 to 10 times by using deionized water and ethanol.
5. The regular polyhedral alpha-Fe of claim 4 2 O 3 FromThe preparation method of the growth material is characterized in that in the step 2), the drying conditions are as follows: drying for 10 to 20 hours at 60 to 80 ℃ in a common way.
6. The regular polyhedral alpha-Fe of claim 5 2 O 3 The preparation method of the self-growing material is characterized in that in the step 4), the washing times are 6 to 10 times by using deionized water and ethanol; the drying conditions were: drying at 60-80 ℃ for 15-20 h.
7. The regular polyhedral alpha-Fe of claim 6 2 O 3 Regular polyhedral alpha-Fe prepared by preparation method of self-growing material 2 O 3 The self-growing material is applied to the field of gas sensors.
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| CN106698522A (en) * | 2016-09-13 | 2017-05-24 | 济南大学 | Preparation method of alpha-Fe2O3 cube and microsphere |
| CN108314089A (en) * | 2018-02-01 | 2018-07-24 | 济南大学 | A kind of porous flower-shaped α-Fe2O3The synthetic method of self-assembled nanometer material |
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|---|---|---|---|---|
| CN104229900A (en) * | 2014-09-15 | 2014-12-24 | 济南大学 | Preparation method of alpha-Fe2O3 cubes |
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