CN108217751A - A kind of preparation method of hexa-prism alpha-FeOOH nano-rod - Google Patents
A kind of preparation method of hexa-prism alpha-FeOOH nano-rod Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01G49/02—Oxides; Hydroxides
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention discloses a kind of preparation method of hexa-prism α FeOOH nanometer rods, with Iron(III) chloride hexahydrate FeCl3·6H2O, polyvinylpyrrolidone (PVP), ammonium fluoride (NH4F) and ammonium hydroxide (25%wt) is raw material, and second alcohol and water is used as solvent, is reacted 6 hours under the conditions of 180 DEG C, obtained monodisperse, high-purity hexa-prism nanometer α FeOOH.Its preparation process is simple compared with prior art by the present invention, it operates nimble, design principle is reliable, production cost is low, and product yield is high, and application environment is friendly, the hexa-prism α FeOOH nanometer rods monodispersities prepared are good, purity is high, is had broad application prospects in terms of lithium ion battery negative material, is easy to carry out large-scale industrial production.
Description
Technical field：
The invention belongs to technical field of nanometer material preparation, are related to a kind of use hydro-thermal reaction method and prepare hexa-prism hydroxyl
The method of base iron oxide (alpha-feooh) nanometer rods, product can be used as the occasions such as electrode material, catalyst and magnetic recording material.
Background technology：
Goethite (alpha-feooh) is to be widely present in nature and one of highly important iron hydroxide, is stabilized
In acid soil, the reaction of the interface interaction and surface oxidation reduction that have plays very heavy during environmental geochemistry
The effect wanted.In modern environment, alpha-feooh can to the organic pollution in air, water body and deposit and heavy metal from
Son is adsorbed and catalysed oxidn, changes their existing forms and their migration, toxicity and ecological effect, because
This nano α-FeOOH material shows superior characteristic in terms of the improvement and reparation of environment；In addition, nano α-FeOOH material
It is nontoxic low with processing cost due to specific capacity height, it is made to have broad application prospects in lithium ion battery negative material.
At present, have many document reports to grind about the preparation method and its microscopic appearance of nanostructured FeOOH
Study carefully.For example, using hydro-thermal method prepare nano wire (M.Fei, et al., J.Am.Chem.Soc., 2011,133,8408-
8411.), nanometer rods (B.Tang, et al., Inorg.Chem., 2006,45,5196-5200.), nanobelt (Z.An, et
Al., Mater.Res.Bull., 2012,47,3976-3982.), nano whiskers (G.N.Subbanna, etal.,
Mater.Chem.Phys., 2003,78,43-50.), flower-shaped (H.F.Chen, et al., J.Mater.Sci:
Mater.Electron., 2011,22,252-259.), air oxidation process prepare hollow microsphere (S.Cao, et al.,
2009,57,2154-2165.) and sol-gel method, chemical precipitation method, microemulsion method etc., but α ActaMater. ,-
Different FeOOH patterns and structure have extremely important influence to its performance, come with regard to 1-dimention nano alpha-feooh microstructure
It says, prepares a kind of nano α-FeOOH of new pattern and have great importance to practical application.At present, about hexa-prism α-
There is not been reported for the preparation and its application of FeOOH nanometer rods, and hexa-prism alpha-feooh is prepared especially with hydro-thermal reaction method
There is not been reported for the technological means of nanometer rods.
Invention content：
The shortcomings that it is an object of the invention to overcome the prior art, seeks design and provides a kind of method using hydro-thermal reaction
The new process of hexa-prism alpha-FeOOH nano-rod is prepared, preparation process is simple, and principle is reliable, and production cost is low, no dirt
Dye, material property are good.
In order to achieve the above-mentioned object of the invention, the method for the present invention is with Iron(III) chloride hexahydrate FeCl3·6H2O, polyvinyl pyrrole
Alkanone (PVP), ammonium fluoride (NH4F) and ammonium hydroxide (25%wt) is raw material, and second alcohol and water is reacted as solvent under the conditions of 180 DEG C
6 hours, be made monodisperse, high-purity hexa-prism nano α-FeOOH, specific process step includes：
(1) by FeCl3·6H2O is dissolved in the mixed solution containing absolute ethyl alcohol and deionized water, is stirred evenly；
(2) PVP is dissolved in the mixed solution containing absolute ethyl alcohol and deionized water, stirred evenly, it is added with dropper
Enter in the solution that step (1) obtains, stir, obtain mixed solution；
(3) ammonium hydroxide is added in the solution that step (2) obtains, stirs, obtain mixed solution；
(4) by ammonium fluoride (NH4F it) is added in deionized water, waits to be completely dissolved, be added to the solution that step (3) obtains
In, stirring obtains mixed solution；
(5) mixed solution that step (4) obtains is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining, 150
It is reacted 3~8 hours at~200 DEG C, obtains yellowish-brown sample；
(6) after the yellowish-brown sample that step (5) obtains is cleaned successively with deionized water and ethyl alcohol, 60 DEG C of drying obtain
Monodisperse hexa-prism alpha-FeOOH nano-rod.
Further, in the step (1) and (2), the volume ratio of absolute ethyl alcohol and deionized water is 1:1.2~1.2:1.
Further, in the step (2), FeCl3·6H2The mass ratio of O and PVP is 27:55, volume ratio 1:1~
1.2。
Further, in the step (3), a concentration of 25%wt of ammonium hydroxide.
Further, in the step (4), the mass ratio of NH4F and deionized water is 7:400..
Wherein, the OH- and Fe3+ that ammonium hydroxide hydrolysis provides forms hydrated ferric oxide in the solution, promotes Fe3+ hydrolysis and shape
Core, surfactant PVP and F- can reduce the surface energy of alpha-feooh crystal particular crystal plane, so as to reach the mesh of control pattern
's.
Compared with prior art, beneficial effects of the present invention are：Its preparation process is simple compared with prior art by the present invention,
Operate nimble, design principle is reliable, and production cost is low, and product yield is high, and application environment is friendly, the hexa-prism α prepared-
FeOOH nanometer rods monodispersity is good, and purity is high, has broad application prospects, is easy in terms of lithium ion battery negative material
Carry out large-scale industrial production.
Description of the drawings：
Fig. 1 is the XRD spectrum of hexa-prism alpha-FeOOH nano-rod prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM image of hexa-prism alpha-FeOOH nano-rod prepared by the embodiment of the present invention 1, wherein (a) bows for SEM
View, (b) are the SEM enlarged drawings at the top of single hexa-prism alpha-feooh.
Fig. 3 is the TEM image and model schematic of hexa-prism alpha-FeOOH nano-rod prepared by the embodiment of the present invention 1,
In (a) be hexa-prism alpha-FeOOH nano-rod bright field image, (b) be hexa-prism alpha-feooh model schematic.
Fig. 4 is the chemical property figure of hexa-prism alpha-FeOOH nano-rod prepared by the embodiment of the present invention 1.
Specific embodiment：
The present invention is further elaborated below by specific embodiment and with reference to attached drawing.
Embodiment 1：
A kind of tool prepares the technique of hexa-prism alpha-FeOOH nano-rod, and specific steps include：
(1) prepared by solution 1：The absolute ethyl alcohol of 13.6mL and 16.3mL deionized waters are mixed, then 0.54g's
FeCl3·6H2O is added in solution, is stirred evenly, and obtains solution 1；
(2) prepared by solution 2：The PVP of 1.1g is dissolved in the absolute ethyl alcohol containing 13.6mL and 16.3mL deionized waters mix
It in solution, stirs evenly, obtains solution 2；
(3) prepared by mixed solution：The solution 2 obtained in step (2) is added drop-wise to dropper in solution 1, is stirred by magnetic force
It mixes, obtains uniformly mixed solution, then the ammonium hydroxide of 105uL is taken to be added drop-wise in mixed solution with liquid-transfering gun, be vigorously stirred 20 minutes,
The 22mL deionized water solutions containing 0.4g NH4F are added drop-wise in mixed solution again, magnetic agitation, obtained uniformly mixed molten
Liquid；
(4) sample preparation：The mixed solution that step (3) obtains is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is reacted 3 hours under the conditions of 200 DEG C of temperature control, obtains solid yellowish-brown sample；
(5) prepared by finished product：The yellowish-brown sample that step (4) is obtained uses deionized water and washes of absolute alcohol three times successively
Afterwards, 60 DEG C of drying of temperature control, obtain monodisperse hexa-prism alpha-FeOOH nano-rod finished product.
The finished product that this example obtains is in X-ray diffractometer (model：Rigaku SmartLab), scanning electron microscope (model：
) and transmission electron microscope (model HitachiS-4800：JEOL JEM2100F) on be detected.Wherein, Fig. 1 be the present embodiment into
Product XRD diffraction patterns, are specifically scanned with the sweep speed of 4 °/min from 20 ° -80 °.By comparing XRD standard cards, this spreads out
It penetrates figure with alpha-feooh to match, the product for showing hexa-prism is alpha-feooh, and Fig. 2 (a) is the vertical view scanning electron microscope of finished product
Figure as can be seen from the figure tests the shape that the alpha-feooh being prepared is in hexagonal prisms, and end has a pointed shape, finished product rib length
Size is 800-900nm, length of side 100nm；Fig. 2 (b) is the single alpha-feooh end scanning electron microscope (SEM) photograph that the present embodiment obtains,
Product can be clearly seen in hexa-prism structure, every stick top is there are two inclined-plane, and inclined-plane is trapezoidal, and Fig. 3 (a) is finished product
Transmission electron microscope picture is overlooked, as can be seen from the figure complete alpha-FeOOH nano-rod；Fig. 3 (b) for ideal hexa-prism α-
FeOOH illustratons of model are made of four trapezoidal bottom surfaces and six sides, and the nanocrystalline direction of growth is [001] direction, with this reality
The angle and profile for applying the hexa-prism alpha-feooh that example is prepared are coincide.
The finished product of the present embodiment is applied in lithium ion battery negative material, and the results are shown in Figure 4 for electrochemical property test.
Under the current density of 200mA/g, after 100 circle charge and discharge cycles, the specific capacity of battery remains able to be stably held in
821mAh/g shows that prepared hexa-prism alpha-FeOOH nano-rod has good follow as lithium ion battery negative material
Ring performance.
Embodiment 2
A kind of tool prepares the technique of hexa-prism alpha-FeOOH nano-rod, and specific steps include：
(1) prepared by solution 1：The absolute ethyl alcohol of 15mL and 15mL deionized waters are mixed, then the FeCl3 0.54g
6H2O is added in solution, is stirred evenly, and obtains solution 1；
(2) prepared by solution 2：The PVP of 1.1g is dissolved in the absolute ethyl alcohol containing 15mL and 15mL deionized water mixed solutions
In, it stirs evenly, obtains solution 2；
(3) prepared by mixed solution：The solution 2 obtained in step (2) is added drop-wise to dropper in solution 1, is stirred by magnetic force
It mixes, obtains uniformly mixed solution, then the ammonium hydroxide of 115 μ L is taken to be added drop-wise in mixed solution with liquid-transfering gun, be vigorously stirred 15 minutes,
The 20mL deionized water solutions containing 0.35g NH4F are added drop-wise in mixed solution again, magnetic agitation obtains uniformly mixed
Solution；
(4) sample preparation：The mixed solution that step (3) obtains is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is reacted 6 hours under the conditions of 180 DEG C of temperature control, obtains solid yellowish-brown sample；
(5) prepared by finished product：The yellowish-brown sample that step (4) is obtained uses deionized water and washes of absolute alcohol three times successively
Afterwards, 60 DEG C of drying of temperature control, obtain monodisperse hexa-prism alpha-FeOOH nano-rod finished product.
Embodiment 3
A kind of tool prepares the technique of hexa-prism alpha-FeOOH nano-rod, and specific steps include：
(1) prepared by solution 1：The absolute ethyl alcohol of 13.6mL and 16.3mL deionized waters are mixed, then 0.54g's
FeCl36H2O is added in solution, is stirred evenly, and obtains solution 1；
(2) prepared by solution 2：The PVP of 1.1g is dissolved in the absolute ethyl alcohol containing 13.6mL and 16.3mL deionized waters mix
It in solution, stirs evenly, obtains solution 2；
(3) prepared by mixed solution：The solution 2 obtained in step (2) is added drop-wise to dropper in solution 1, is stirred by magnetic force
It mixes, obtains uniformly mixed solution, then the ammonium hydroxide of 125 μ L is taken to be added drop-wise in mixed solution with liquid-transfering gun, be vigorously stirred 25 minutes,
The 18mL deionized water solutions containing 0.3g NH4F are added drop-wise in mixed solution again, magnetic agitation, obtained uniformly mixed molten
Liquid；
(4) sample preparation：The mixed solution that step (3) obtains is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is reacted 8 hours under the conditions of 150 DEG C of temperature control, obtains solid yellowish-brown sample；
(5) prepared by finished product：The yellowish-brown sample that step (4) is obtained uses deionized water and washes of absolute alcohol three times successively
Afterwards, 60 DEG C of drying of temperature control, obtain monodisperse hexa-prism alpha-FeOOH nano-rod finished product.
Claims (7)
1. a kind of preparation method of hexa-prism alpha-FeOOH nano-rod, it is characterised in that specific steps include：
(1) mixed solution A containing absolute ethyl alcohol and deionized water is configured；
(2) by Iron(III) chloride hexahydrate (FeCl3·6H2O mixed solution A) is dissolved in, is uniformly mixed and obtains solution 1；
(3) polyvinylpyrrolidone (PVP) is dissolved in mixed solution A, is uniformly mixed and obtains solution 2；
(4) solution 2 is added drop-wise in solution 1, stirs, obtain mixed solution；
(5) ammonium hydroxide is added in the solution that step (4) obtains, stirs, obtain mixed solution；
(6) by ammonium fluoride (NH4F it) is dissolved in deionized water, waits to be completely dissolved, be added in the solution that step (5) obtains, stir,
Obtain mixed solution；
(7) mixed solution that step (6) obtains is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining, 150~200
It is reacted 3~8 hours at DEG C, product obtains hexa-prism alpha-FeOOH nano-rod after over cleaning, drying.
2. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod according to claim 1, which is characterized in that described
The volume ratio of absolute ethyl alcohol and deionized water is 1 in step (1):1.2~1.2:1.
3. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod according to claim 1, which is characterized in that described
FeCl in step (2)3·6H2O is 1 with deionized water quality ratio in solution A:25~1:31.
4. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod according to claim 1, which is characterized in that described
FeCl in step (2) and (3)3·6H2The mass ratio of O and PVP is 27:55.
5. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod according to claim 1, which is characterized in that described
Ammonium hydroxide and deionized water volume ratio in solution A are 1 in step (5):130.
6. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod according to claim 1, which is characterized in that described
FeCl in step (6)3·6H2O and NH4The mass ratio of F is 54:30~54:40.
7. the preparation method of a kind of hexa-prism alpha-FeOOH nano-rod described in accordance with the claim 1, which is characterized in that described
NH in step (6)4F and the mass ratio of deionized water are 7:400.
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| CN201810135090.3A CN108217751B (en) | 2018-02-09 | 2018-02-09 | Preparation method of hexagonal prism α -FeOOH nanorod |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115092968A (en) * | 2022-06-08 | 2022-09-23 | 中国石油大学(华东) | Preparation method, product and application of iron oxyhydroxide catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103432969A (en) * | 2013-09-09 | 2013-12-11 | 青岛科技大学 | Preparation method of alpha-Fe2O3/FeOOH core-shell structure composite microspheres |
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| US20160083410A1 (en) * | 2013-09-25 | 2016-03-24 | Korea Institute Of Energy Research | Metal oxalate hydrate body having a certain shape, preparation method thereof, and metal oxide/carbon composite body prepared from the same |
| CN107500363A (en) * | 2017-08-16 | 2017-12-22 | 青岛大学 | A kind of preparation method of prism hexa-prism nano-sized iron oxide |
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2018
- 2018-02-09 CN CN201810135090.3A patent/CN108217751B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103432969A (en) * | 2013-09-09 | 2013-12-11 | 青岛科技大学 | Preparation method of alpha-Fe2O3/FeOOH core-shell structure composite microspheres |
| CN103446965A (en) * | 2013-09-09 | 2013-12-18 | 青岛科技大学 | Preparation method of nickel-doped alpha-Fe2O3 multi-level structure spinous microspheres |
| US20160083410A1 (en) * | 2013-09-25 | 2016-03-24 | Korea Institute Of Energy Research | Metal oxalate hydrate body having a certain shape, preparation method thereof, and metal oxide/carbon composite body prepared from the same |
| CN107500363A (en) * | 2017-08-16 | 2017-12-22 | 青岛大学 | A kind of preparation method of prism hexa-prism nano-sized iron oxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115092968A (en) * | 2022-06-08 | 2022-09-23 | 中国石油大学(华东) | Preparation method, product and application of iron oxyhydroxide catalyst |
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