KR100733331B1 - Method of making nano MPP powder using RF plasma combustion - Google Patents

Abstract

The present invention nano-powdered micro-size MPP (MPP) powder using RF Plasma combustion technology, which is excellent in soft magnetic properties, which is a material shielding electromagnetic waves and magnetic fields in an electromagnetic harmful environment, and mixed with a resin The present invention relates to a method for manufacturing nano MPP powder by RF plasma combustion technology that can produce a thin sheet-like sheet or apply or deposit on a transparent film to shield harmful electromagnetic waves and magnetic fields and impart a heat shielding function at the same time. . The present invention can manufacture MPP micropowders as nanopowders to produce electromagnetic shielding, heat shielding, and functional films or ultra-thin pads having these functions. The present invention relates to RF plasma (RF) in an inert gas atmosphere chamber. Plsama), and then dozens of micro MPP (MPP) powders are added, and high purity nano powders prepared by vaporization and condensation are collected and applied or deposited on a thin transparent film to shield electromagnetic waves and heat-transparent transparent films. It provides a nano MPP powder manufacturing method by the RF plasma combustion technology to be produced.

MPP micro powder, nano powder, functional transparent film, electromagnetic shielding, heat shield.

Description

Method of making nano MPP powder by RF plasma combustion technology

1 is a schematic configuration diagram of an RF plasma combustion apparatus of the present invention;

2 is a flow chart of nanoparticles manufacturing of RF plasma combustion apparatus;

3 is an XRD graph confirming the presence of MPP,

4 is a TEM photograph showing the presence and particle size of the MPP,

5 is a graph of particle size distribution experiment results showing the MPP particle size,

6 is a graph showing the results of evaluation of magnetic properties of MPP nanopowders;

Figure 7 is a graph of the magnetic properties evaluation results after the MPP nano powder heat treatment.

<Description of Major Symbols in Drawing>

20: powder supply part, 22: central gas part (central gas),

24: sheath gas (sheath gas),

26: RF plasma torch,

The present invention is nano-powdered using the RF plasma (RF Plasma) combustion technology of micro-sized MPP (Moly Permalloy Powder) powder having excellent soft magnetic properties, which is a material that shields electromagnetic waves and magnetic fields in an electromagnetic harmful environment, The nano MPP powder is manufactured by RF plasma combustion technology that can be mixed with resin to form a thin thin sheet or apply or deposit on a transparent film to shield harmful electromagnetic waves and magnetic fields and impart heat shielding function simultaneously. It is about a method.

In general, Permalloy is a general term for high permeability materials such as 35-80% Ni-Fe binary alloy and multi-alloy alloys in which Mo, Cu, Cr and the like are added thereto. After Elme et al. Obtained a high permeability by quenching 78% Ni Permalloy at 600 ° C in 1916, Mo, Cr, Cu, etc. were added, and the composition range showing good characteristics was almost confirmed in the 1930s. It can be seen.

Since then, the characteristics have been improved according to the advancement of manufacturing technology such as high purity hydrogen atmosphere heat treatment and vacuum melting, for example, supermalloy. In addition, isoperm using rolling magnetic anisotropy, Permenorm 5000 Z using texture, and recently, Permax Z, Satmumetal, Permax F, which control induced magnetic anisotropy (uniaxial magnetic anisotropy) Kinds of materials are being produced.

Interest in the so-called Permalloy problem of permalloy-related phenomena, that is why Permalloy exhibits a high permeability, has been studied to identify the cause of high permeability. As the contents of this study, the study on the regular lattice, and the mechanism explanation for the induced magnetic anisotropy caused by cooling or cold rolling in the magnetic field was attempted.

Since 1960, research has been carried out on ultra-high permeability materials such as Mo-based Permalloy and Ni-Fe binary Permalloy having high permeability. Since then, the development of permalloy with high wear resistance and high degree for magnetic head has been proceeded.

These MPPs have high permeability and high square ratios, and are attracting attention as energy conversion and amplification, low and high frequency iron cores, low and high frequency generators, magnetic amplifiers, magnetic memory circuits, various sensors, and recently, MRAM materials. In addition, it is applied as a material for shielding electromagnetic waves or magnetic fields in the environment of harmful electromagnetic waves. A sheet or pad made of a thin sheet or a powder mixed with micro powder and resin of 1 t or less has a harmful function to a device or a human body. It is used in various ways to shield the electromagnetic waves and magnetic fields.

However, with the recent increase in the harmful environment of the electromagnetic wave, many people have increased their awareness of this and the development of materials to shield them is increasing day by day. There is a need for a material capable of being applied to a transparent film and having transparency, an electromagnetic wave shielding material having a function, a material capable of shielding an external heat source, and a material that can be manufactured with ultra-thin sheets and capable of the aforementioned function.

MPP is manufactured in the form of a sheet or made of several micro powders, and the sheet is bent or processed according to a target object, and in the case of powder, it is mixed with a resin to form a pad. To shield electromagnetic and magnetic fields. By the way, such a sheet (pad) or pad (pad), the transparency is not secured in order to manufacture in the form of ultra-thin, another high integration technology is required.

The present invention, which solves the above-mentioned problems, is made by nanoparticles by MPP micropowder, and by nanoparticles by RF plasma combustion technology, which can produce transparent film or pad having electromagnetic shielding, thermal barrier, and such function. It is an object to provide a method for producing MPP powder.

The present invention generates RF plasma (RF Plsama) in the inert gas atmosphere chamber, and then dozens of micro MPP (MPP) powder is added to the high purity nano-powder prepared by the process of vaporization and condensation to collect on a thin transparent film It is an object of the present invention to provide a method for producing nano MPP powder by RF plasma combustion technology for coating or depositing an electromagnetic wave shielding and heat shielding transparent film.

Nano-MPP powder manufacturing method by RF plasma combustion technology of the present invention to achieve the above-mentioned object, and the first step of supplying MPP (MPP) powder of 10 ~ 100 micro size or less through the nozzle inside the RF plasma torch unit and After adjusting the plasma power of the RF to generate a plasma to control the flow rate, speed and type of the gas is injected , and the third step to vaporize or dissolve the MP powder by heating at a high temperature in the RF plasma torch unit And, in step 4, condensation or quenching of the MPP powder by quenching gas to produce nano MPP powder, and 5 steps of separating large nanoparticles from the nano MPP powder and collecting them through a filter, and on the outer wall of the filter. When the nanopowder is adsorbed, the backflush in the filter includes six steps of recovering the nano MPP powder. All.

In addition, in the second step, the present invention is to put the MPP micro powder ( sample ) into the powder supply unit, and to control the plasma plasma power to 15-150kW to generate a plasma, to form an inert gas atmosphere in the chamber, Inert gas and hydrogen are mixed with the amount of the sheath gas in the gas injected around the plasma torch, and the amount of the inert gas is 10-120 slpm, and the amount of hydrogen gas is 10-50 slpm, Nano-MPP powder is added using 5-40 slpm of inert gas, 5-40 slpm of inert gas, 50-400 slpm of inert gas, and quenching gas. It characterized in that it comprises the preparation.

In addition, the present invention is characterized in that the center of the induction coil and the height spacing to generate the RF (RF) and the lower end of the metallic nozzle of the RF plasma torch to within 3cm, and the nano-MPP powder produced under the optimum heat treatment conditions vacuum After the heat treatment in the middle and then mixed with the resin to produce a pad or coated or deposited on a transparent film, characterized in that the production of a functional film or functional pad having a function of electromagnetic shielding and heat shielding in the form.

In addition, the parameters for determining the particle size of the MPP powder prepared are RF plasma power, the height of the metallic nozzle and the induction coil for generating the RF, the radius of the metallic nozzle, the supply amount and speed of the micro-size MPP powder, It is characterized by the amount of quenching gas and the like.

Hereinafter, a method of manufacturing nano MPP powder by RF plasma combustion technology of the present invention will be described in detail with reference to the accompanying drawings.

1 is a schematic configuration diagram of an RF plasma combustion apparatus of the present invention, FIG. 2 is a flowchart illustrating a nano powder production of the RF plasma combustion apparatus, and FIG. 3 is an XRD graph confirming the presence of MPP. 4 is a TEM photograph showing the presence and the particle size of the MPP, Figure 5 is a graph of the particle size distribution experiment showing the particle size of the MPP, Figure 6 is a graph of the magnetic properties evaluation results of the MPP nanopowder, Figure 7 is an MPP nano powder heat treatment After the magnetic property evaluation results graph.

1 is a block diagram of an RF plasma combustion apparatus, and includes a powder supply unit 20, a central gas unit 22, a sheath gas unit 24, and an RF plasma unit. A torch portion (RF plasma torch) 26, quench gas portion 30, filter 32, nano powder collecting portion 34, the outer tube 36 and the like.

RF plasma torch (26) generates a plasma by RF and serves to lengthen the diameter and length of the flame. The gas is injected to the outer wall of the nozzle into which the micro powder is injected, and the sheath gas 24 is injected to prevent the vaporized powder from adsorbing to the outer wall of the induction coil, which is an RF generator. A carrier gas for transferring MPP micro powder is provided.

If the injected BMP blood (MPP) micro powder reached a plasma (plasma) the flame temperature of the plasma generated by the induction loop plasma torch (Induction plasma torch) forms a high-temperature environment of about 5,000 ~ 10,000 K powder is liquefied It is then vaporized or dissolved .

At this time, the RF plasma torch portion (RF plasma torch) 26 (plasma torch) is condensed or quenched by a quenching gas (quenching gas) that is strongly injected through the quench gas portion 30 at the lower end is nano-powdered.

The produced nanopowder is transported by a vacuum pump or compressor, passes through a cyclone 28, the temperature of the powder is lowered, the nanopowder is collected in a filter 32, and the gas is Out through the outer tube (36).

When a predetermined amount is adsorbed on the outer wall of the filter 32 , the back is flushed inside the filter and the nano powder is desorbed and recovered from the bottom of the nano powder container. Nanopowders have a very large surface area in contact with the reactable gas, so care must be taken in recovery and treatment.

Carrier gas , central gas, sheath gas, and quenching gas in the lower part of the induction plasma torch. The amount and velocity of the gas determine the particle size distribution of the nanopowder, and in particular, the optimum conditions need to be established because the type of sheath gas has a great influence on the temperature distribution of the plasma flame.

FIG. 2 is a view illustrating a process of preparing nanopowders, illustrating a location of a gas to be injected when RF plasma treatment is performed in an inert gas atmosphere, a process of separating the micropowder and the nanopowder, and a final collection process. .

The collected MPP nanopowder is applied directly onto the transparent film, or mixed with a dispersant and deposited on the transparent film to have a uniform distribution, thereby producing a functional film capable of electromagnetic shielding and heat shielding.

An embodiment of the present invention will be described.

Precursors for synthesizing MPP nanopowders using RF plasma equipment used MPP powders of 10 to 100 microns in size or less.

The MPP micro powder was placed in a powder feeder 20 and rotated at a speed of 20 RPM and 20% vibration was applied to the sample through a nozzle inside the RF plasma torch 26. Supply.

RF plasma power (RF Plasma power) was adjusted to 50kW to generate a plasma, and then the flow rate, speed, and type of each gas to be injected were adjusted.

The parameters that determine the particle size of MPP nanopowders are RF plasma power, metallic nozzles that supply a precursor to the torch, and induction coils that generate RF. And the height of the metal, the radius of the metallic nozzle, the amount and speed of the precursor supply, and the amount of quenching gas to quench the vaporized or dissolved specimen.

The height distance between the lower end of the mentioned metallic nozzle and the center of the induction coil generating RF is controlled within 3 cm.

In addition, whether the MPP nanopowder is accurately formed or whether impurities are formed in the second or third phase may be classified into three kinds of gases, which are made of inert gas and plasma torch , inside the RF plasma torch unit 26. Gas is determined by the sheath gas (central gas), the central gas (central gas), the carrier gas (carrier gas).

The following table summarizes the synthetic conditions for the production of MPP nanopowders.

                   table. 1 Nano MPP Synthesis Conditions Condition Plasma Power  50 kW   Gas Sheath Ar: 100 H ₂ : 20 Central Ar: 20 slpm Quenching Ar: 200 slpm Carrier Ar: 20 slpm

MPP micron powder is synthesized into MPP nano powder through pyrolysis and regrowth by high temperature of plasma. It was confirmed by the XRD whether the phase of the nano-powder collected through the filter 32 and the presence of the second phase, the results are illustrated in FIG.

 3 shows the crystal structure of the MPP nanopowder through XRD diffraction analysis, in which the MPP crystal phase is the main crystal phase and no second phase is observed.

Figure 4 is an example of the TEM image showing the presence and the particle size of the MPP, it was looked through the TEM and particle size analyzer to determine whether the crystal phase is a nano state.

As illustrated in FIG. 4, the particles had a size of 100 nm or less and had a spherical shape.

5 is a graph of particle size distribution experiment showing the particle size of the MPP, the particle size was analyzed by the particle size analyzer, it was determined that the average size of 100 nm.

Magnetic properties are very important because MPP nanopowder will be used for electromagnetic shielding.

FIG. 6 is a graph illustrating the results of evaluation of the magnetic properties of the MPP nanopowders. As a result of comparison with the magnetic properties of the micro MPP powders, it was confirmed that nano MPP powders having no significant change in magnetic properties were prepared.

7 is a graph showing the results of evaluation of magnetic properties after heat treatment of MPP nanopowders. As a result of evaluating the magnetic properties after heat treatment between 550-800 degrees in a vacuum heat treatment furnace, the heat treatment temperature is increased in the range of 550-800 degrees. As a result, the permeability increased and the maximum susceptibility increased.

MPP nanopowders prepared by the above-described RF plasma combustion technique of the present invention were heat-treated in a vacuum heat treatment furnace and mixed with a resin to prepare ultra-thin pads to shield electromagnetic waves. The shielding results were shown, and the result of evaluation of electromagnetic shielding rate, heat shielding rate and transparency by coating or depositing on transparent film showed good characteristics.

While the invention described above has been shown and described with respect to particular embodiments, it has been described by way of example only to illustrate the invention and is not intended to limit the invention to the embodiments described above. Those skilled in the art will appreciate that various modifications and changes of the present invention can be made without departing from the spirit and scope of the invention as set forth in the claims below. The present invention intends to make clear that all such modifications and variations are included within the scope of the present invention.

As described above, the present invention nano-powdered MPP micro powder using RF plasma combustion technology, which has excellent soft magnetic properties, which is a material shielding electromagnetic waves and magnetic fields in an electromagnetic environment, and using nano powder. By mixing with the resin to produce a sheet (thin sheet) in the form of a thin film or coated on a transparent film or deposited to shield the harmful electromagnetic waves and magnetic fields, it can be produced a functional film or ultra-thin pad (pad) with a heat shield function.

Claims (6)

Supplying MPP powder having a size of 10-100 micrometers or less through the nozzle to the inside of the RF plasma torch; Controlling the plasma power of the RF to generate plasma and controlling the flow rate, velocity, and type of the gas to be introduced; Heating and heating at a high temperature in an RF plasma torch unit to vaporize or dissolve the MPP powder after liquefying ; Condensing or quenching the MPP powder by a quenching gas to produce nano MPP powder; Separating five nanoparticles from the nano MPP powder and collecting the same through a filter; When the nano-powder is adsorbed on the outer wall of the filter, the back-flush in the filter to recover the nano MPP powder, characterized in that it comprises a nano MPP powder by RF plasma combustion technology, characterized in that it comprises a six steps. The method of claim 1, In the second step, MPP micro powder is placed in the powder supply section and the specimen is supplied, and plasma is generated by adjusting the RF plasma power to 15-150 kW, and then an inert gas atmosphere is formed in the chamber, and around the plasma torch The amount of sheath gas in the input gas is mixed with inert gas and hydrogen, but the amount of inert gas is 10-120 slpm, the amount of hydrogen gas is 10-50 slpm, and the central gas is inert. 5-40 slpm as gas, 5-40 slpm as carrier gas, and 50-400 slpm as quench gas as inert gas to produce nano MPP powder. Nano MPP powder production method by RF plasma combustion technology. The method of claim 1, The method of manufacturing nano MPP powder by RF plasma combustion technology comprising adjusting the distance between the bottom of the metallic nozzle of the RF plasma torch and the induction coil center and the height spacing generating RF (RF) within 3 cm. delete delete The method of claim 1, Variables for determining the particle size of the MPP powder prepared are RF plasma power, the height of the metallic nozzle and the induction coil generating the RF, the radius of the metallic nozzle, the supply amount and speed of the micro sized MPP powder, and the quenching gas. Method for producing nano MPP powder by RF plasma combustion technology, characterized in that determined by the amount of .

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