CN101704557A - Preparation method of beta-FeOOH nano-wire - Google Patents
Preparation method of beta-FeOOH nano-wire Download PDFInfo
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- CN101704557A CN101704557A CN200910213167A CN200910213167A CN101704557A CN 101704557 A CN101704557 A CN 101704557A CN 200910213167 A CN200910213167 A CN 200910213167A CN 200910213167 A CN200910213167 A CN 200910213167A CN 101704557 A CN101704557 A CN 101704557A
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Abstract
The invention discloses a preparation method of a beta-FeOOH nano-wire, relating to the technical field of production processes of an inorganic nano-material. The preparation method comprising the following steps of: firstly, preparing an n-butyl alcohol solution of ferric chloride and ureal; adding sodium dodecyl benzene sulfonate to the n-butyl alcohol solution; placing into an enclosed reactor; completing an reaction at 70 +/-2 DEG C; and naturally cooling to room temperature and obtaining the beta-FeOOH nano-wire; wherein the concentration of the sodium dodecyl benzene sulfonate in the n-butyl alcohol solution is 0-0.5 mM. The beta-FeOOH nano-wire prepared by the method is a claybank solid with anti-ferromagnetic property and is a spindle-shaped granule in an aqueous solution. By adding the sodium dodecyl benzene sulfonate with different concentrations, the invention can produce the beta-FeOOH nano-wire with consistent diameter and adjustable length.
Description
Technical field
The present invention relates to a kind of technical field of producing of inorganic nano material, particularly a kind of preparation method of one dimension beta-FeOOH nano-wire.
Background technology
Monodimension nanometer material is one of member important in the nano material extended familys.The scientific worker generally believes that it is the idealized system of physical propertiess such as research electronic transport character, optical characteristics, magnetic property and mechanics mechanical property, will occupy extremely important status in the development process of unicircuit such as nano electron device, opto-electronic device and field-effect transistor and functional element.Since Iijima (S.lijima) professor in 1991 found carbon nanotube, monodimension nanometer material had caused numerous areas scientist's very big concern.In the past few years, the nano material that is reported in of the synthetic aspect of relevant one dimension Nano structure has occupied absolute majority in synthetic, and people are making great efforts most of solid matters are all grown into (standard) one dimension Nano structure.Calendar year 2001, because the distinguished service of monodimension nanometer material research particularly has been assembled into circuit with it, this makes people see a brand-new world.In order to satisfy the needs of theoretical investigation and practical application, the controlled preparation of the size of monodimension nanometer material, phase purity, degree of crystallinity and chemical ingredients just becomes particularly important.Other method of comparing has characteristics such as easy to operate, low-cost industrialization but the control of the liquid phase of monodimension nanometer material is synthetic, thereby causes scientific worker's extensive interest, also will have huge economic benefit.
Summary of the invention
Purpose of the present invention just is to develop a kind of method for preparing beta-FeOOH nano-wire simple, that cost is low for preparing.
Technical scheme of the present invention comprises the steps:
1) butanol solution of preparation iron trichloride and urea, wherein, the mol ratio of iron trichloride and urea is 6: 1.
2) add Sodium dodecylbenzene sulfonate in described butanol solution, put into airtight reactor, reaction naturally cools to room temperature to finishing under 70 ± 2 ℃ of temperature condition, obtains beta-FeOOH nano-wire; The concentration that contains Sodium dodecylbenzene sulfonate in the described butanol solution is 0mM～5.0mM.
β-the FeOOH (Akagan é ite) that adopts the inventive method to make has anti-ferromagnetic pale brown look solid, belongs to oblique system (a=1.056nm, b=0.3031nm, c=1.0483nm, β=90.63 °), the I2/m spacer.β-FeOOH is a kind of semiconductor material (band gap 2.12eV) simultaneously.Can be used for redox reaction and coal hydrogenation catalyst for reaction, preparation γ-Fe
2O
3And α-Fe
2O
3Raw material, and the preparation lithium cell the iron-based active material.The general fusiformis β-FeOOH particle that obtains in the aqueous solution.
It is solvent that characteristics of the present invention are used propyl carbinol exactly, by adding the anion surfactant (dodecyl sodium sulfonate is received) of different concns, can produce constant substantially, the length-adjustable beta-FeOOH nano-wire of diameter.Produce raw materials used commonly, required production unit is few, and operation steps is simple, mild condition, product size evenly, good dispersity is suitable for industrial production.
Advantage of the present invention and effect are that production cost is low, so than suitability for industrialized production.Has wide market application prospect.
In addition, raw material of the present invention adopts the iron trichloride that contains six crystal water, and purpose is the raw material convenience, is easy to get, and helps industrial production.
Description of drawings
Fig. 1 is the photo of the prepared beta-FeOOH nano-wire of the embodiment of the invention 1.
Fig. 2 is the x-ray diffraction pattern of the prepared beta-FeOOH nano-wire product of the embodiment of the invention 1.
Fig. 3 is the transmission electron microscope photo figure of the prepared β-FeOOH powder-product of the embodiment of the invention 1.
Fig. 4 is the transmission electron microscope photo figure of the prepared beta-FeOOH nano-wire product of the embodiment of the invention 2.
Fig. 5 is the transmission electron microscope photo figure of the prepared beta-FeOOH nano-wire product of the embodiment of the invention 3.
Embodiment
Embodiment 1:
1, takes by weighing iron trichloride 0.2021g (0.750mmol) and the urea 0.0074g (0.125mmol) that contains six crystal water respectively, be dissolved in simultaneously in the 50ml propyl carbinol.
2, above-mentioned solution adding is furnished with in the water heating kettle of polytetrafluoroethylliner liner, behind 70 ℃ of reaction 5h, stops heating, make it naturally cool to room temperature.
3, by centrifugal, filtration, washing, obtain solid phase prod.
As Fig. 1, Fig. 2 and shown in Figure 3.The photo of solid phase prod is taken by Canon's 610 type digital cameras.German Bruker AXS D8 ADVANCE X-ray powder diffraction instrument (XRD, Cu K are adopted in the structure of product and the thing identification of phases
αRadiation, λ=1.54056
40kV 200mA) measures.Adopt JEM-2000EX type transmission electron microscope that the pattern and the granular size of product are observed.
Test-results shows:
Fig. 1: the embodiment of the invention 1 has prepared pale brown look solid phase prod.
Fig. 2: the x-ray diffraction pattern of the embodiment of the invention 1 products made thereby.Its all X-ray diffraction peaks from left to right correspond respectively to (200), (310), (400), (211), (301), (411), (600), (521), (002) and (541) crystal face of β-FeOOH, illustrate that embodiment 1 products made thereby is high-purity beta-FeOOH.
Fig. 3: the transmission electron microscope photo of the embodiment of the invention 1 made β-FeOOH product.From this figure as can be known, made β-FeOOH product is a nano wire, length 130nm～160nm, particle diameter 3nm～5nm.Length-to-diameter ratio 26～53.
Embodiment 2:
1, takes by weighing iron trichloride 0.2021g (0.750mmol) and the urea 0.0074g (0.125mmol) that contains six crystal water respectively, be dissolved in simultaneously in the 50ml propyl carbinol.
2, in above-mentioned butanol solution, adding anion surfactant---Sodium dodecylbenzene sulfonate makes the concentration of Sodium dodecylbenzene sulfonate in solution reach 1.0mM.
3, above-mentioned solution adding is furnished with in the water heating kettle of polytetrafluoroethylliner liner, behind 70 ℃ of reaction 5h, stops heating, make it naturally cool to room temperature.
4, by centrifugal, filtration, washing, obtain solid phase prod.
The photo of solid phase prod is taken by Canon's 610 type digital cameras.German BrukerAXS D8 ADVANCE X-ray powder diffraction instrument (XRD, Cu K are adopted in the structure of product and the thing identification of phases
αRadiation, λ=1.54056
40kV 200mA) measures.Adopt JEM-2000EX type transmission electron microscope that the pattern and the granular size of product are observed.
Test-results shows:
The prepared solid phase prod of the embodiment of the invention 2 is identical with embodiment 1 products obtained therefrom, all is pale brown look solid.
The x-ray diffraction pattern of the x-ray diffraction pattern of the embodiment of the invention 2 products made therebies and embodiment 1 products made thereby is identical.Illustrate that embodiment 2 products made therebies are high-purity beta-FeOOH.
Fig. 4: the transmission electron microscope photo of the embodiment of the invention 2 made β-FeOOH products.From this figure as can be known, made β-FeOOH product is a nano wire, length 60nm～90nm, particle diameter 3nm～5nm.Length-to-diameter ratio 12～30.
Embodiment 3:
1, takes by weighing iron trichloride 0.2021g (0.750mmol) and the urea 0.0074g (0.125mmol) that contains six crystal water respectively, be dissolved in simultaneously in the 50ml propyl carbinol.
2, in above-mentioned butanol solution, adding anion surfactant---Sodium dodecylbenzene sulfonate makes the concentration of Sodium dodecylbenzene sulfonate in solution reach 5.0mM.
3, above-mentioned solution adding is furnished with in the water heating kettle of polytetrafluoroethylliner liner, behind 70 ℃ of reaction 5h, stops heating, make it naturally cool to room temperature.
4, by centrifugal, filtration, washing, obtain solid phase prod.
The photo of solid phase prod is taken by Canon's 610 type digital cameras.German BrukerAXS D8 ADVANCE X-ray powder diffraction instrument (XRD, Cu K are adopted in the structure of product and the thing identification of phases
αRadiation, λ=1.54056
40kV 200mA) measures.Adopt JEM-2000EX type transmission electron microscope that the pattern and the granular size of product are observed.
Test-results shows:
The prepared solid phase prod of the embodiment of the invention 5 is identical with embodiment 1 products obtained therefrom, all is pale brown look solid.
The x-ray diffraction pattern of the x-ray diffraction pattern of the embodiment of the invention 5 products made therebies and embodiment 1 products made thereby is identical.Illustrate that embodiment 2 products made therebies are high-purity beta-FeOOH.
Fig. 5: the transmission electron microscope photo of the embodiment of the invention 3 made β-FeOOH products.From this figure as can be known, made β-FeOOH product is a nano wire, length 40nm～60nm, particle diameter 3nm～5nm.Length-to-diameter ratio 8～20.
Conclusion:
According to above-mentioned result of study as can be known: the inventive method can be used fairly simple experimental technique under comparatively gentle condition, it is constant substantially to have synthesized diameter, length-adjustable beta-FeOOH nano-wire.
Claims (2)
1. the preparation method of a beta-FeOOH nano-wire is characterized in that following steps:
1) butanol solution of preparation iron trichloride and urea, wherein, the mol ratio of iron trichloride and urea is 6: 1.
2) add Sodium dodecylbenzene sulfonate in described butanol solution, put into airtight reactor, reaction naturally cools to room temperature to finishing under 70 ± 2 ℃ of temperature condition, obtains beta-FeOOH nano-wire; The concentration that contains Sodium dodecylbenzene sulfonate in the described butanol solution is 0mM～5.0mM.
2. according to the preparation method of the described beta-FeOOH nano-wire of claim 1, it is characterized in that described iron trichloride is the iron trichloride that contains six crystal water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204548A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH |
| CN108505319A (en) * | 2018-05-04 | 2018-09-07 | 辽宁大学 | A kind of environment-friendly type super hydrophobic material and its preparation method and application |
| CN108927101A (en) * | 2018-07-06 | 2018-12-04 | 济南大学 | A kind of acicular nanometer FeOOH adsorbent and preparation method thereof |
| CN109499523A (en) * | 2018-11-28 | 2019-03-22 | 北京工业大学 | A kind of FeOOH/MnO2The preparation method of@diatomite composite material |
-
2009
- 2009-10-19 CN CN200910213167A patent/CN101704557A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204548A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH |
| CN103204548B (en) * | 2013-04-12 | 2014-10-01 | 陕西科技大学 | Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH |
| CN108505319A (en) * | 2018-05-04 | 2018-09-07 | 辽宁大学 | A kind of environment-friendly type super hydrophobic material and its preparation method and application |
| CN108927101A (en) * | 2018-07-06 | 2018-12-04 | 济南大学 | A kind of acicular nanometer FeOOH adsorbent and preparation method thereof |
| CN109499523A (en) * | 2018-11-28 | 2019-03-22 | 北京工业大学 | A kind of FeOOH/MnO2The preparation method of@diatomite composite material |
| CN109499523B (en) * | 2018-11-28 | 2021-11-05 | 北京工业大学 | FeOOH/MnO2Preparation method of @ diatomite composite material |
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Open date: 20100512 |