Method for extracting nano second phase by using non-aqueous solution electrolysis system

Abstract

The invention relates to a method for extracting a nano second phase by using a non-aqueous solution electrolysis system and application thereof. Through the unique design of the electrolysis system,an electrolyte solution forms overflow and eddy current in the electrolysis process, the overflow and eddy current electrolyte solution continuously scours an electrode and an electrolytic cell, and the adsorption of the nano second phase on the surfaces of the electrode and the electrolytic cell and the agglomeration of the nano second phase can be effectively prevented. Through electrolyte solution component design, especially cooperative use of an electrolyte, a thickening agent and a complexing agent, selective electrolytic reaction of the ferromagnetic alloy can be realized, effective separation of a matrix and a second phase in the ferromagnetic alloy is realized, and sedimentation and coating of Fe<3+> on the surface of the second phase are inhibited; the sedimentation resistance ofthe second phase is effectively increased and the sedimentation of the second phase is inhibited. By using the electrolyte solution and the electrolysis system, the electrolytic reaction efficiency can be improved, the collection rate of the second phase with a size smaller than 20nm, especially the collection rate of the second phase with a size smaller than 15nm is increased, and extraction andcharacterization of the nano second phase in the ferromagnetic alloy are achieved.

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 ...

AI Technical Summary

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

Images