A method for extracting nanometer second phase by using non-aqueous solution electrolysis system

Abstract

The invention relates to a method for extracting a nanometer second phase by using a non-aqueous solution electrolysis system and its application. The invention uses a unique design of the electrolysis system to make the electrolyte form overflow and eddy current during the electrolysis process, and the overflow and eddy current electrolyte continuously washes the electrodes and the electrolytic cell, which can effectively prevent the second nano-phase from forming in the electrode and the electrolytic cell. Surface adsorption and agglomeration of nanosecond phases. Through the design of electrolyte composition, especially the combined use of electrolyte, thickener and complexing agent, the selective electrolysis reaction of ferromagnetic alloy can be realized, the effective separation of matrix and second phase in ferromagnetic alloy can be realized, and the Fe 3+ Settling and covering on the surface of the second phase; effectively increasing the second phase settling resistance and inhibiting the second phase settling. The use of the electrolyte solution and electrolysis system is beneficial to improving the efficiency of the electrolysis reaction, improving the collection rate of the second phase with a size smaller than 20nm, especially smaller than 15nm, and realizing the extraction and characterization of the nanometer second phase in the ferromagnetic alloy.

Description

technical field [0001] The invention relates to a method for extracting a nanometer second phase by using a non-aqueous solution electrolysis system, which belongs to the fields of electrochemistry and material characterization. Background technique [0002] Second phase strengthened ferromagnetic alloys are an important class of alloy materials. Accurate characterization of micro- and nanoscale second phases in ferromagnetic alloys is an important way to design and develop high-performance ferromagnetic alloys and their preparation technologies. Metallographic microscopes and scanning electron microscopes cannot completely characterize the structure and lattice sequence of the micro- and nanoscale second phases, especially the nano-scale second phases. Analysis and characterization, and the preparation of high-quality TEM / HRTEM test samples is an important prerequisite for accurate characterization of alloys. [0003] At present, the main preparation methods of TEM / HRTEM ...

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Problems solved by technology

[0006] (1)Y 2 o 3 It is easy to react and dissolve in hydrochloric acid, and it is easy to make Y 2 o 3 , especially nano Y 2 o 3 The structure of the phase is destroyed, and the sample preparation conditions are harsh; Fe 3+ Easily hydrolyzed to form Fe(OH) 3 Colloid or precipitation, which settles and covers the surface of the second phase particles, contaminating the sample;

[0007] (2) The above-mentioned electrolyte and its use also have the following problems: 1. The electrolytic reaction rate and efficiency are low; 2. The second phase separated by the electrolytic reaction, especially the second phase particles with a size less than 20nm, is easily adsorbed on the electrodes and the electrolytic cell The surface of the wall, and it is not easy to desorb, which leads to the distortion of the information of the second phase particles, especially the information of the second phase particles whose size is less than or equal to 10nm, and the basic processing is completely distorted; Solve this problem fundamentally; ④The large-size second phase has low sedimentation resistance and is easy to settle during the electrolysis process. Using the above-mentioned electrolyte will easily cause part of the large-size settlement and loss, which will eventually lead to the loss of information about the large-size second phase. Completely reflect the information of the second phase;

[0008] (3) When filter paper is used to separate inclusions in steel, due to the limitation of the pore size of the filter paper, nanoscale particles are also easily lost during the filtration process; at the same time, the second nano-phase is easily adsorbed on the surface and pores of the filter paper, resulting in Part of the second phase is missing; when the second phase is collected by centrifugation, since the nano second phase is not easy to settle, it is easy to cause the loss of nano second phase information

[0009] In short, ferromagnetic alloys have strong magnetism, and the TEM / HRTEM test samples prepared by conventional methods are fragile and easy to fall off, and there is a potential risk of damage to the electron microscope; the second phase information is incomplete, which is difficult for the preparation of ferromagnetic alloy TEM / HRTEM samples. and the great difficulty of accurately characterizing

When the second phase is extracted by the acid solution method, Y 2 o 3 It is easy to react chemically in hydrochloric acid, and the sample preparation conditions are harsh; Fe 3+ The ions will form Fe(OH) 3 Colloids or precipitates cover the surface of the second phase particles and contaminate the sample; when separated by physical methods such as filtration and centrifugation, the nanoscale second phase is easily lost, and the prepared samples cannot completely reflect the information of the second phase in the alloy

The second phase separated by the current electrolysis technology, especially the second phase with a size smaller than 20nm, is easy to adsorb on the electrode surface, and the second phase with a large size is easy to settle. There are long electrolysis time, low efficiency, and incomplete information about the second phase with a small size. And other issues

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