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Preparation of one-dimensional Fe3O4 nano-needle material having modulated structure

A nano-needle and conductive metal technology, applied in nano-materials and nano fields, can solve problems such as difficult and stable physical phases, and achieve the effects of low equipment requirements, high degree of controllability and good reproducibility

Inactive Publication Date: 2008-10-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high temperature (above 450 ° C) oxidation environment Fe 3 o 4 The phase is difficult to exist stably, and there is no synthesis of one-dimensional Fe under high-temperature oxidation conditions. 3 o 4 Research report on nanomaterials
However, no one-dimensional Fe with modulated structure has been prepared by high-temperature thermal oxidation. 3 o 4 Research report on nanomaterials

Method used

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  • Preparation of one-dimensional Fe3O4 nano-needle material having modulated structure
  • Preparation of one-dimensional Fe3O4 nano-needle material having modulated structure
  • Preparation of one-dimensional Fe3O4 nano-needle material having modulated structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A 1D Fe with modulated structure 3 o 4 The preparation method of nanoneedle material, it comprises the steps:

[0029] 1) Dissolve ferrous chloride, boric acid, saccharin and sodium fluoride in distilled water, then adjust the pH value to 2.0 by adding dilute sulfuric acid or sodium hydroxide aqueous solution dropwise, prepare an electrolyte solution, and place it in a Hull cell; Mix per liter of electrolyte: ferrous chloride 380g, boric acid 20g, saccharin 5g, sodium fluoride 2.5g; (note: the volume is determined by a standard Hull cell with a capacity of 267ml, when the volume of electrolyte required by the Hull cell is 1 Timing, the amount of ferrous chloride, boric acid, saccharin, sodium fluoride, distilled water can be determined);

[0030] 2) Using the pulse electrodeposition technology, adopt the pulse electrodeposition parameters with the output pulse frequency f of 50-500Hz, the duty cycle r of 5-50%, the positive pulse working current of 0.3-0.5A, and the n...

Embodiment 2

[0040] Embodiment 2: (research the one-dimensional Fe prepared by different thermal oxidation time 3 o 4 Changes in morphology and microstructure of nanoneedle materials):

[0041] The preparation is basically the same as in Example 1, except that the nanocrystalline Fe film is heated at 900° C. in air for 3 hours, and the SEM photo of the scanning electron microscope is shown in Figure 2b .

[0042] to combine Figure 2a , Figure 2b Explanation: The SEM photo of the synthesized product shows that when the thermal oxidation time exceeds 30 minutes, the morphology and density of the thermal oxidation product no longer change significantly.

Embodiment 3

[0047] A 1D Fe with modulated structure 3 o 4 The preparation method of nanoneedle material, it comprises the steps:

[0048] 1) Dissolve ferrous chloride, boric acid, saccharin and sodium fluoride in distilled water, then adjust the pH value to 2.0 by adding dilute sulfuric acid or sodium hydroxide aqueous solution dropwise, prepare an electrolyte solution, and place it in a Hull cell; For each liter of electrolyte: 380g of ferrous chloride, 20g of boric acid, 5g of saccharin, 2.5g of sodium fluoride;

[0049] 2) Adopt the pulse electrodeposition technology, adopt the pulse electrodeposition parameters of output pulse frequency f as 50Hz, duty ratio r as 5%, positive pulse working current 0.3A, negative pulse working current 0.1A; place the conductive metal substrate in the storage In the Hull cell with the electrolyte of step 1), the conductive metal substrate is connected to the cathode of the power supply, the anode of the power supply is connected to the standard anode,...

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Abstract

The invention relates to a preparation method of one-dimensional Fe3O4 nanoneedle material provided with a modulated structure. The preparation method of the one-dimensional Fe3O4 nanoneedle material provided with the modulated structured is characterized in that the preparation method comprises the steps that firstly, ferrous chloride, boric acid, saccharin and sodium fluoride are dissolved into distilled water, and then the pH value is adjusted to 2.0 by dripping weak sulphuric acid or sodium hydroxide solution to be prepared into electrolyzed solution to be positioned in a hull cell; 380 g of ferrous chloride, 20 g of boric acid, 5 g of saccharin and 2.5 g of sodium fluoride are prepared in the electrolyzed solution per liter; secondly, the pulse galvanic depositing technology is adopted, and the pulse galvanic depositing parameter with output pulse frequency f of 50 to 500 Hz, duty factor r of 5 to 50 percent, positive pulse operating current of 0.3 to 0.5 A and negative operating current of 0.1 to 0.3A is adopted; a conductive metal base plate is positioned in the hull cell, the pulse galvanic depositing is lasted for 3 to 20 minutes, and a layer of nanocrystalline Fe thin film is electrically deposited on the surface of the conductive metal base plate; thirdly, the nanocrystalline Fe thin film is heated for 0.5 to 3 hours at 900 DEG C, to obtain the one-dimensional Fe3O4 nanoneedle material provided with t modulated structure. The method has the advantages that the process is simple, the controllable degree is high, the preparation method conforms to the environment requirement, and the cost is low.

Description

technical field [0001] The invention belongs to the field of nanomaterials and nanotechnology, in particular to a one-dimensional Fe with a modulation structure 3 o 4 Preparation methods of nanoneedle materials. Background technique [0002] Ferromagnetic nanomaterials can be widely used in magnetic storage materials and devices. Among many ferromagnetic materials, magnetite Fe 3 o 4 It is the most famous and important ferromagnetic material in the ferrite family. Fe 3 o 4 With an inverse spinel structure, one of the Fe 3+ ion takes the A site, the other Fe 3+ and an Fe 2+ Recombined at the B site, at room temperature electrons can be in the Fe at the B site 3+ and Fe 2- transition between ions, making Fe 3 o 4 Become a very important semi-metallic magnetic material, which can be widely used in the fields of pigments, catalysts, cold storage and magnetic storage devices. [0003] At present, the vast majority of research has focused on the magnetite Fe 3 o 4 ...

Claims

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Application Information

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IPC IPC(8): C25D3/20C25D5/00C23C8/14C23F17/00
Inventor 刘曰利陈文钟蕾李洪全舒威周静
Owner WUHAN UNIV OF TECH
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