CN115259235A - Simple synthesis method of three-dimensional ferric oxide with haystack structure formed by stacking nano short rods - Google Patents
Simple synthesis method of three-dimensional ferric oxide with haystack structure formed by stacking nano short rods Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000001308 synthesis method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 19
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims abstract description 17
- 239000001433 sodium tartrate Substances 0.000 claims abstract description 17
- 229960002167 sodium tartrate Drugs 0.000 claims abstract description 17
- 235000011004 sodium tartrates Nutrition 0.000 claims abstract description 17
- 239000002073 nanorod Substances 0.000 claims abstract description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 41
- 239000003446 ligand Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 16
- 239000004005 microsphere Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 3
- 235000013980 iron oxide Nutrition 0.000 description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 11
- 238000003756 stirring Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- 229940032296 ferric chloride Drugs 0.000 description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 230000001788 irregular Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000002608 ionic liquid Substances 0.000 description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 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
- 238000000137 annealing Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 iron alkoxide Chemical class 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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]
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/32—Spheres
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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
- C01P2004/50—Agglomerated particles
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a simple synthesis method of three-dimensional ferric oxide with a haystack structure formed by stacking nano short rods. According to the method, sodium tartrate and ferric nitrate are used as reaction raw materials, deionized water is used as a solvent, and in a specific synthesis process, the synthesis of the nano iron oxide structures with different structures and appearances can be controlled by changing the experimental conditions such as the ratio of the amount of sodium tartrate to the amount of ferric salt, the reaction temperature and the like. The three-dimensional ferric oxide with the haystack structure is formed by stacking a large number of nano rods with different lengths, is similar to haystack in shape and has higher strength (the three-dimensional structure is not easy to collapse in the reaction process); in addition, the nanorods are stacked with each other to form a large number of pore channel structures, which is beneficial to the diffusion of reaction substances in the material. The synthesis method has the advantages of simplicity, convenience, low price, rapidness, environmental friendliness, controllable material appearance and the like, and can be used for selectively and controllably synthesizing the nano ferric oxide three-dimensional material with different appearances and structures according to actual needs.
Description
Technical Field
The invention relates to a simple synthesis method of three-dimensional ferric oxide with a haystack structure formed by stacking nano short rods, belonging to the technical field of inorganic material synthesis.
Background
As one of inorganic functional materials, the iron oxide has the advantages of stable structure, acid and alkali resistance, high temperature resistance, environmental friendliness, no toxicity, low price and the like, so that the iron oxide has a good application prospect in the fields of coatings, lithium batteries, sensors, photocatalysts, biomedical treatment and the like, and attracts the close attention of researchers. The iron oxide three-dimensional structure has larger surface area and space pore channels, can provide more reaction sites for reaction, and shorter ion diffusion channels, and the like, thereby causing wide attention of scientific research personnel. The iron oxide three-dimensional structures reported at present are more, and hollow spheres, nanoflowers and nanoneedle arrays are common in the structures, but the iron oxide three-dimensional structures which are stacked by the nano short rods and are shaped like haystack as mentioned in the invention are not reported.
The three-dimensional structures of iron oxides that have been reported in recent years are mainly: liu and the like take sodium acetate and ferric chloride hexahydrate as raw materials, ethylene glycol as a solvent, a flower-like iron alkoxide precursor is prepared by adopting a method of stirring at a constant temperature of 150 ℃ for 52 hours, and then the precursor is calcined in air at a temperature of 500 ℃ for 1 hour to obtain a porous flower-like iron oxide microsphere structure (P.Liu, J.J.guang, W.Rui, a novel chemical material, 47 (2019) 161-165). Chen et al use Fe (NO)3And C6H12N4The self-assembled iron oxide submicron sphere structure (Y.C.Chen, K.Zhang, Y.G.Zhao, inorganic chemistry report, 25 (2009) 2003-2009) is prepared by using ethylene glycol as a solvent and adopting a method of solvent heat treatment at 160 ℃ for 8h and subsequent high-temperature calcination. Wang et al prepared an iron oxide microsphere structure assembled from nanosheets by a quasi-emulsion method using ferrous sulfate heptahydrate as an iron source, water and glycerol as solvents (b.wang, j.s.chen, h.b.wu, et al, journal of the American Chemical Society,133 (2011) 17146-17148). Xie and the like take sodium sulfate and ferric chloride hexahydrate as raw materials, and a hollow microsphere iron oxide structure assembled by nanorods is prepared by adopting a mode of combining hydrothermal treatment at 140 ℃ for 12 hours and hydrothermal treatment at 600 ℃ for 2 hours (X.L.Xie, H.Q.Yang, H.Jiao, et al., chinese science (chemistry), 38 (2008) 595-606). Cao et al utilize K3[Fe(CN)6]The hydrothermal reaction of hydrolysis produced three-dimensional dendritic iron oxide nanostructures (m.h.cao, t.f.liu, s.gao, et al, angelw Chem Int Ed,44 (2005) 4197-4201). Zhong et al prepared iron oxide microsphere structures assembled from nanosheets by using ferric chloride and urea as raw materials, using a glycol solution containing tetrabutylammonium bromide as a solvent, and adopting 190 ℃ solvothermal treatment and subsequent high-temperature calcination treatment (l.s.zhong, j.s.hu, h.p.liang, et al, adv Mater,18 (2006) 2426-2431). Chinese patent 201710437760.2 discloses a method for polycondensing dicyandiamide containing ferric chloride and formaldehyde by using FTO conductive glass as a substratePreparing a nanorod array precursor in an aqueous solution, and then calcining at a high temperature to prepare the iron oxide nanorod array. Chinese patent 201811090873.0 discloses an ionic liquid Gemini (Gemini) imidazole surfactant [ C ] with ferric chloride hexahydrate as an iron source12-2-C12im]Br2The method for preparing the ferric oxide nano-microsphere by combining high-temperature hydrothermal treatment with a subsequent high-temperature calcination process is adopted as an auxiliary reagent. Chinese patent 201811264859.8 discloses a method for preparing iron oxide hollow porous microspheres by taking ferric salt, ionic liquid and ethylene glycol as raw materials and utilizing a solvothermal method and a subsequent calcination treatment method. Chinese patent 201710142202.3 discloses a method for preparing an iron oxide nanorod array by using a titanium sheet as a substrate, using ferric chloride and sodium sulfate as raw materials and combining a hydrothermal method and a high-temperature sintering method. Chinese patent 201710098112.9 discloses a method for preparing an iron oxide nanoneedle array by taking a ceramic tube as a base, taking ferric chloride and sodium sulfate as raw materials and adopting a hydrothermal method and an annealing treatment process. The related method for preparing the three-dimensional structure of the ferric oxide has complicated process, needs to use a template, a substrate, ionic liquid, a surfactant, an organic solvent or a structure directing agent and the like, so that the preparation process has higher cost and more uncontrollable factors to influence the final appearance and structure of the product, and easily pollutes the environment by using an organic reagent. Therefore, it is necessary to find a method for preparing the iron oxide three-dimensional structure, which is simple and easy to implement, low in cost, controllable in conditions and environment-friendly.
Disclosure of Invention
The invention aims to provide a simple synthesis method of three-dimensional iron oxide with a haystack structure, which is formed by stacking nano short rods. The invention takes sodium tartrate and ferric nitrate nonahydrate as reaction raw materials and deionized water as a solvent. In the specific synthesis process, the synthesis of the nano iron oxide structures with different structures and appearances can be controlled by changing the ratio of the amount of the sodium tartrate to the amount of the ferric salt, the reaction temperature, the reaction time and other experimental conditions. The three-dimensional iron oxide with the haystack structure is formed by stacking a large number of nano rods with different lengths, is shaped like a haystack and has higher strength (the three-dimensional structure is not easy to collapse in the reaction process); in addition, the nanorods are stacked to form a large number of pore channel structures, which is beneficial to the diffusion of the reaction substances in the material. The synthesis method has the advantages of simplicity, convenience, low price, rapidness, environmental friendliness, controllable material morphology and the like, and can be used for selectively and controllably synthesizing the nano iron oxide three-dimensional material with different morphologies and structures according to actual needs.
The technical scheme of the invention is as follows: a simple synthesis method of three-dimensional ferric oxide with a haystack structure formed by stacking nano short rods is characterized in that ferric nitrate is used as an iron source, sodium tartrate is used as a ligand, and deionized water is used as a solvent to prepare the ligand and Fe3+The solution with the mass ratio of 1.5 is then synthesized into the three-dimensional ferric oxide with the haystack structure by a hydrothermal method at 135-145 ℃ and stacked by nano short rods.
Furthermore, the three-dimensional iron oxide structure formed by stacking the nano short rods is formed by stacking a large number of nano rods with different lengths, wherein the nano rods are about tens of nanometers (10-100 nanometers) wide and about several micrometers (1-10 micrometers) long; the three-dimensional structure is shaped like a stack of grass and has greater strength (the three-dimensional structure is not easy to collapse during the reaction process). The nanorods of the structure are stacked mutually to form a large number of pore channel structures, which is beneficial to the diffusion of reaction substances in the material.
Preferably, the preparation method specifically comprises the following steps:
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as a ligand and deionized water as a solvent3+The solution with the mass ratio of 1.5 is ultrasonically stirred at normal temperature to form a mixed solution;
2) Transferring the mixed solution obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 140 ℃ for reaction for 12 hours;
3) And after the reaction is finished, centrifugally collecting a product, washing, and drying in the air to obtain the three-dimensional iron oxide haystack structure stacked by the nano short rods.
Further, the drying is as follows: air dried at 80 ℃ for 6 hours.
Further, the washing is as follows: washed 3 times with deionized water and absolute ethanol, respectively.
The invention also discloses a simple synthesis method of the solid microsphere structure three-dimensional ferric oxide, which is characterized in that a ligand and Fe3+The quantity ratio of the substances is 1.0, and the rest steps and conditions are the same as those of the method for synthesizing the three-dimensional ferric oxide with the haystack structure.
The invention also discloses a simple synthesis method of the irregular-structure three-dimensional ferric oxide, which is characterized in that the hydrothermal reaction temperature is 120 ℃, and the rest steps and conditions are the same as those of the synthesis method of the three-dimensional ferric oxide with the haystack structure.
The invention also discloses a simple synthesis method of the three-dimensional ferric oxide with the rod-shaped structure, which is characterized in that the hydrothermal reaction temperature is 160 ℃, and the rest steps and conditions are the same as those of the synthesis method of the three-dimensional ferric oxide with the haystack structure.
By adopting the technical scheme, the invention has the technical effects that:
1. compared with the reported technology, the method uses sodium tartrate and the like as raw materials, has the advantages of low raw material price, simple and easy synthesis process, rapidness, environmental friendliness and the like, and can realize modulation of the product micro-morphology and structure by modulating synthesis conditions (the quantity ratio of the ligand to the iron source substance, the reaction time of a reaction system, the reaction temperature and the like) (three-dimensional iron oxide haystack structure stacked by nano short rods, nano particle accumulation bodies, solid microsphere structures, irregular particles, rod-shaped structures and the like can be sequentially prepared according to the change of specific experimental conditions).
2. Particularly, the three-dimensional iron oxide haystack structure formed by stacking the nano short rods prepared by the method can be formed at one time under the condition of no template, and the three-dimensional structure is not easy to deform and damage and can provide more possibilities for the subsequent application; in addition, the nanorods are stacked to form a large number of pore channel structures, which is beneficial to the diffusion of the reaction substances in the material.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a three-dimensional iron oxide haystack structure formed by stacking nano short rods at 20000 times;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a three-dimensional iron oxide haystack structure formed by stacking nano short rods at a magnification of 10000 times;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of a three-dimensional iron oxide haystack structure formed by stacking nano short rods at 5000 times;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a nanoparticle stack;
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of a solid microsphere structure;
FIG. 6 is a Scanning Electron Microscope (SEM) photograph of irregular particles;
fig. 7 is a Scanning Electron Microscope (SEM) photograph of the rod-like structure.
Detailed Description
The following examples are provided to further illustrate the invention and are not intended to be limiting. The volume of the deionized water is 12mL, and the addition amount of the ferric nitrate nonahydrate is 0.0012mol.
Example 1
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+Ultrasonically stirring the solution with the mass ratio of 1.5 at normal temperature for 20min to form a brown yellow transparent solution;
2) Transferring the mixed system obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 140 ℃ for reaction for 12 hours;
3) After the reaction is finished, centrifuging and collecting a product, washing the product for 3 times by using deionized water and absolute ethyl alcohol respectively, and then drying the product for 6 hours in the air at the temperature of 80 ℃;
4) And taking the dried sample for phase state and appearance characterization analysis. The scanning electron microscope test result shows that: the obtained product has obvious three-dimensional structure (shaped like a haystack), and the structure is formed by stacking a large number of nanorods with different lengths and widths of about tens of nanometers and lengths of about several micrometers; the three-dimensional structure, such as a stack, has greater strength (the three-dimensional structure does not collapse easily during the reaction). The nanorods of the structure are mutually stacked to form a large number of pore channel structures, which is beneficial to the diffusion of reaction substances in the material. The three-dimensional nanostructure has good stability, and can maintain the original three-dimensional structure after repeated grinding (see fig. 1-3).
Example 2
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+Ultrasonically stirring the solution with the mass ratio of 0.5 at normal temperature for 20min to form a brown yellow transparent solution;
2) Transferring the mixed system obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 140 ℃ for reaction for 12 hours;
3) After the reaction is finished, centrifuging and collecting a product, washing the product for 3 times by using deionized water and absolute ethyl alcohol respectively, and then drying the product for 6 hours in the air at the temperature of 80 ℃;
4) And taking the dried sample for phase state and morphology characterization analysis. Scanning electron microscope test results show that the obtained product is a nano-particle accumulation body, and the size of the nano-particle accumulation body is small, and the agglomeration is serious (see figure 4).
Example 3
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+Ultrasonically stirring the solution with the mass ratio of 1.0 at normal temperature for 20min to form a brown yellow transparent solution;
2) Transferring the mixed system obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 140 ℃ for reaction for 12 hours;
3) After the reaction is finished, centrifuging and collecting a product, washing the product for 3 times by using deionized water and absolute ethyl alcohol respectively, and then drying the product for 6 hours in the air at the temperature of 80 ℃;
4) And taking the dried sample for phase state and appearance characterization analysis. The scanning electron microscope test result shows that the obtained product is a solid microsphere structure which has larger volume, smooth surface and good dispersibility (see figure 5).
Example 4
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+The mass ratio of the substances is 1.5Ultrasonically stirring the solution for 20min at normal temperature to form a brown yellow transparent solution;
2) Transferring the mixed system obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 120 ℃ for reaction for 12 hours;
3) After the reaction is finished, centrifuging and collecting a product, washing the product for 3 times by using deionized water and absolute ethyl alcohol respectively, and then drying the product for 6 hours in the air at the temperature of 80 ℃;
4) And taking the dried sample for phase state and morphology characterization analysis. The scanning electron microscope test results showed that the resulting product had an irregular structure with a certain degree of dispersion (see FIG. 6).
Example 5
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+Ultrasonically stirring the solution with the mass ratio of 1.5 at normal temperature for 20min to form a brown yellow transparent solution;
2) Transferring the mixed system obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 160 ℃ for reaction for 12 hours;
3) After the reaction is finished, centrifuging and collecting a product, washing the product for 3 times by using deionized water and absolute ethyl alcohol respectively, and then drying the product for 6 hours in the air at the temperature of 80 ℃;
4) And taking the dried sample for phase state and morphology characterization analysis. The scanning electron microscope test result shows that the obtained product has a rod-shaped structure, the size distribution of the structure is wide, and irregular particles exist on the surface of part of the rod-shaped structure (see figure 7).
Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. Stacked nano short rodA simple synthesis method of three-dimensional ferric oxide with a haystack structure is characterized in that ferric nitrate is used as an iron source, sodium tartrate is used as a ligand, and deionized water is used as a solvent to prepare the ligand and Fe3+The solution with the mass ratio of 1.5 is then synthesized into the three-dimensional ferric oxide with the haystack structure by a hydrothermal method at 135-145 ℃ and stacked by nano short rods.
2. The method for simply synthesizing the three-dimensional iron oxide with the haystack structure by stacking the nano short rods as claimed in claim 1, wherein the three-dimensional iron oxide with the haystack structure is formed by stacking a large number of nano rods with different lengths, the width of which is 10-100 nanometers and the length of which is 1-10 micrometers; the three-dimensional structure is formed as a stack of grass.
3. The simple synthesis method of the three-dimensional iron oxide with the haystack structure formed by stacking the nano short rods as claimed in claim 1 or 2, which is characterized by comprising the following steps:
1) Preparing a ligand and Fe by using ferric nitrate nonahydrate as an iron source, sodium tartrate as the ligand and deionized water as a solvent3+The solution with the mass ratio of 1.5 is ultrasonically stirred at normal temperature to form a mixed solution;
2) Transferring the mixed solution obtained in the step 1) into a self-pressure hydrothermal reaction kettle, sealing, and placing in a high-temperature oven at 140 ℃ for reaction for 12 hours;
3) And after the reaction is finished, centrifugally collecting a product, washing, and drying to obtain the three-dimensional ferric oxide with the haystack structure stacked by the nano short rods.
4. The simple synthesis method of the three-dimensional iron oxide with the haystack structure formed by stacking the nano short rods as claimed in claim 3, characterized in that the drying is as follows: air dried at 80 ℃ for 6 hours.
5. The simple synthesis method of the three-dimensional iron oxide with the haystack structure formed by stacking the nano short rods as claimed in claim 3, characterized in that the washing comprises the following steps: washed 3 times with deionized water and absolute ethanol, respectively.
6. A simple synthesis method of solid microsphere structure three-dimensional iron oxide is characterized in that ferric nitrate is used as an iron source, sodium tartrate is used as a ligand, deionized water is used as a solvent, and the ligand and Fe are prepared3+The solid micron sphere structure three-dimensional ferric oxide is synthesized by a hydrothermal method at 140 ℃ after the solution with the mass ratio of 1.0.
7. A simple synthesis method of irregular-structure three-dimensional iron oxide is characterized in that iron nitrate is used as an iron source, sodium tartrate is used as a ligand, and deionized water is used as a solvent to prepare the ligand and Fe3+The solution with the mass ratio of 1.5 is used for synthesizing the irregular-structure three-dimensional ferric oxide by a hydrothermal method at 120 ℃.
8. A simple synthesis method of three-dimensional iron oxide with a rod-shaped structure is characterized in that iron nitrate is used as an iron source, sodium tartrate is used as a ligand, and deionized water is used as a solvent to prepare the ligand and Fe3+The solution with the mass ratio of 1.5 is used for synthesizing the three-dimensional ferric oxide with the rod-shaped structure by a hydrothermal method at 160 ℃.
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