CN109719303A - A kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials - Google Patents
A kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials Download PDFInfo
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- CN109719303A CN109719303A CN201811621105.3A CN201811621105A CN109719303A CN 109719303 A CN109719303 A CN 109719303A CN 201811621105 A CN201811621105 A CN 201811621105A CN 109719303 A CN109719303 A CN 109719303A
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Abstract
The present invention provides a kind of submicron order iron-nickel alloy powder producing methods of soft magnetic materials, in the high-temperature evaporator being sequentially communicated, vapour condenser, it is carried out in the system of powder catcher composition, specific step is as follows: by iron, nickel pure metal raw material is according to certain mass than being put into the close crucible in high-temperature evaporator, after examining the air-tightness of equipment qualified, with the air in inert gas replacement system, light plasma gun, by iron, nickel raw material is melted to heating and vapor state, adjust the throughput of inert gas, by iron, nickel mixed vapour is brought into vapour condenser, iron, nickel mixed vapour is through supercooling, mutually collision, it grows up and finally condenses out, finally it is collected in powder catcher；The characteristics of submicron order FeNi powders of this method production, have crystal grain tiny, and sintering temperature is low, oxygen content is low, complete ball-type, uniform particle sizes, alloying component are evenly distributed, maximum feature is can be with the FeNi powders of large-scale production submicron order.
Description
Technical field
The present invention relates to soft magnetic materials raw material production technical field, specifically a kind of iron-nickel alloy for soft magnetic materials
The preparation method of powder.
Background technique
Electromagnetic interference caused by electromagnetic radiation and electromagnetic problem, which have become, leads to the main of electronic device trouble or failure
Reason.The normal operation of electronic device is not only interfered in electromagnetic radiation, also causes to endanger to personnel's health in radiation areas
Evil, and low frequency magnetic field interference is more scabrous problem in electromagnetic protection field.With the hair at full speed of hyundai electronics information technology
How exhibition prevents and treats electromagnetic radiation and has become a vital step in electronic device manufacture.
The shielding of low frequency magnetic field is to carry out branch to magnetic field using the material of high magnetic permeability, and the magnetic line of force is concentrated on shielding material
Material is internal, and the magnetic field strength of shielding area is reduced with this.Iron nickel alloy film has very excellent soft magnetic characteristic, corrosion-resistant spy
Property, electrology characteristic and mechanical property, be largely used in the storage device of computer and the memory of electronics industry, recording device and
On the electromagnetic shielding of electronic device.With the micromation of electronic circuit and device, integrated, lightweight, it is suitable for electromagnetic shielding
The alloyed powder of iron nickel alloy film not require nothing more than oxygen content low, ingredient is qualified, more and more producers seek it is ultra-fine very
To the FeNi powders for being submicron order.
Summary of the invention
The present invention provides a kind of sub-micro of soft magnetic materials to solve above-mentioned existing deficiencies in the technology
Meter level iron-nickel alloy powder producing method, under high temperature will iron, nickel metal melt, evaporation and obtain after condensing uniform particle sizes it is tiny, at
Divide uniform submicron order FeNi powders.
The technical scheme is that a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials, feature
Be, be sequentially communicated high-temperature evaporator, vapour condenser, powder catcher composition system in carry out, specifically include with
Lower step:
(1) by iron, nickel pure metal raw material according to certain mass than being put into the close crucible in high-temperature evaporator, inspection is set
After standby air-tightness is qualified, the air inlet on high-temperature evaporator and vapour condenser is opened, while opening air-introduced machine, use indifferent gas
Air in body exchange system makes in system to be finally anaerobic or micro- oxygen atmosphere；
(2) plasma gun being mounted in high-temperature evaporator is lighted by high frequency oscillation, generation superhigh temperature electric arc, which is used as, to be added
Heat source continues to heat up by iron, nickel raw material to molten state is heated, and makes to generate iron, nickel mixed vapour above crucible, meanwhile, pass through
Charging system persistently launches iron, nickel raw material into close crucible, to guarantee continuous production；
(3) throughput for adjusting inert gas, iron, nickel mixed vapour is brought into vapour condenser, iron, nickel mixed vapour
Through supercooling, mutually collide, growing up finally condenses out, formed Fe-Ni Alloy Powder；
(4) Fe-Ni Alloy Powder in vapour condenser enters powder catcher with inert gas, then receives toward powder
Gas-solid separator in storage is filled with inert gas, focuses on the iron-nickel alloy of gas-solid separator outer wall higher than powder catcher
In the collection hopper of bottom, gas solid separation is realized, inert gas is recycled under the action of air-introduced machine.
Specifically, iron, nickel mass ratio be 1:1-4；Iron, nickel can be pure metal mechanical mixture, be also possible in proportion
Prefabricated metal block.
Specifically, system pressure 50-120kPa.The pressure size of system is different according to each metal saturated vapour pressure herein
And be adjusted, the pressure of system is reduced, the saturated vapour pressure of iron, nickel can be reduced, is conducive to the evaporation of iron, nickel, is made prepared
Alloy powder component it is more uniform.
Specifically, the plasma gun in high-temperature evaporator is untransferable arc, and the working gas of plasma gun is nitrogen, hydrogen
Or ammonia etc., the power of plasma gun are 60-100kW；Plasma can also be the higher transferred arc of temperature, it is possible to provide up to
The heating power of 130kW.
Specifically, inert gas is nitrogen or argon gas.
Specifically, vapour condenser be gather cold pipe, the structure for gathering cold pipe be followed successively by from inside to outside graphite-pipe, carbon felt pipe,
Carbon felt pipe, stainless steel tube, stainless steel tube, wherein being provided with cold water circulating system between two layers of stainless steel tube.It is condensed by steam
The water flow of cold water circulating system in device can control the cooling velocity of alloyed powder in vapour condenser, and then control alloyed powder
Partial size.
Specifically, by adjusting the throughput size of inert gas in high-temperature evaporator, controllable alloy vapor enters steaming
The flow velocity of the speed of gas condenser and the alloy vapor in vapour condenser, and the size and shape of alloy powder are controlled in turn
The throughput of shape, i.e. inert gas is bigger, and alloy particle is shorter in the time that vapour condenser is grown up, and the partial size of formation is smaller.
Specifically, submicron order FeNi powders average grain diameter is 0.15-0.80 μm, and shape is ball-type.
Specifically, the gas-solid separator in step (4) powder catcher is multiple, and the setting of multiple gas-solid separators makes to close
The collection at bronze end is more effective.
Compared with prior art, the present invention produces the submicron order iron-nickel alloy of soft magnetic materials using vaporize-condensation law
Powder method, have following remarkable advantage and the utility model has the advantages that
1) plasma gun is lighted using high frequency oscillation, generates superhigh temperature electric arc as heating source, iron, nickel raw material is added
Heat melts, dissolves each other, and under the action of plasma arc injection, then the uniform aluminium alloy of forming component increases the function of plasma gun
Rate, the uniform iron-nickel alloy steam of forming component；
2) alloy vapor in entire reaction process in a highly dispersed state, under closed inert gas system protection,
It ensure that the high-purity, high sphericity, the Gao Chengfen uniformity, low oxygen content, the work of biggish surface of submicron order FeNi powders
Property；
3) by controlling the flow of the power of plasma gun, the flow of system. Inert gas, cold water circulating system cooling water,
The submicron order FeNi powders of various particle sizes can be produced, alloyed powder partial size can be controlled in 0.15-0.80 μm, also controllable
The yield of submicron order FeNi powders processed；
4) system use 50-120kPa negative pressure, the fusing point, boiling point and saturated vapour pressure of iron nickel can be reduced, be conducive to iron,
The evaporation of nickel keeps prepared alloy powder component more uniform, while reducing energy consumption；
5) using the submicron order FeNi powders of evaporation-condensation principle production, have crystal grain tiny, sintering temperature is low,
The characteristics of oxygen content is low, complete ball-type, uniform particle sizes, alloying component are evenly distributed, maximum feature is can be with large-scale production
The FeNi powders of submicron order.
Detailed description of the invention
Fig. 1 is that the SEM of two sub-micron grade FeNi powders of embodiment schemes；
Fig. 2 is the EDS figure of nickel in two sub-micron grade FeNi powders of embodiment；
Fig. 3 is the EDS figure of iron in two sub-micron grade FeNi powders of embodiment.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
The raw material that prefabricated iron-nickel alloy mass ratio is 1:3 is added in evaporator in crucible and in charger,
Raw material height on crucible along concordant.The leakproofness of system is checked respectively in negative pressure and direct draught, guarantees system in production not
Gas leakage.Then each cooling water is opened, air-introduced machine is opened, and passes through argon gas, system pressure 90kPa into system.Detection system
Oxygen content it is qualified after, open plasma gun, start to heat raw material.Power is 85kW, and the working gas of plasma gun is argon
Gas and hydrogen.By adjusting the amount of argon inert gas and the power of plasma gun to adjust partial size, finally obtaining partial size is
0.55 μm of FeNi powders, the content of iron are 23%.
Embodiment 2
The raw material that prefabricated iron-nickel alloy mass ratio is 1:1 is added in evaporator in crucible and in charger,
Raw material height on crucible along concordant.The leakproofness of system is checked respectively in negative pressure and direct draught, guarantees system in production not
Gas leakage.Then each cooling water is opened, air-introduced machine is opened, and leads to argon gas, system pressure 90kPa into system.Detection system
Oxygen content it is qualified after, open plasma gun, start to heat raw material.Power is 100kW, and the working gas of plasma gun is argon
Gas and hydrogen.By adjusting the amount of argon inert gas and the power of plasma gun to adjust partial size, finally obtaining partial size is
0.68 μm of FeNi powders, such as Fig. 1, the content of iron are 46%.Fig. 2 and Fig. 3 is that the present embodiment submicron order iron nickel closes respectively
The EDS of nickel and iron schemes in bronze, wherein the white point in Fig. 2 is nickel element, the white point in Fig. 3 is ferro element, can be obvious
Find out that the distribution of nickel and ferroalloy ingredient is very uniform in ground.
Claims (6)
1. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials, which is characterized in that in the high temperature being sequentially communicated
It is carried out in the system that evaporator, vapour condenser, powder catcher form, specifically includes the following steps:
(1) iron, nickel pure metal raw material, than being put into the close crucible in high-temperature evaporator, are examined into equipment according to certain mass
After air-tightness is qualified, the air inlet on high-temperature evaporator and vapour condenser is opened, while opening air-introduced machine, set with inert gas
The air in system is changed, makes in system to be finally anaerobic or micro- oxygen atmosphere；
(2) it lights the plasma gun being mounted in high-temperature evaporator by high frequency oscillation, generates superhigh temperature electric arc as heating source,
Iron, nickel raw material are heated to molten state, continue to heat up, makes to generate iron, nickel mixed vapour above crucible, meanwhile, pass through charging
System persistently launches iron, nickel raw material into close crucible, to guarantee continuous production；
(3) throughput for adjusting inert gas, iron, nickel mixed vapour are brought into vapour condenser, and iron, nickel mixed vapour pass through
It cools down, mutually collide, growing up finally condenses out, formation Fe-Ni Alloy Powder；
(4) Fe-Ni Alloy Powder in vapour condenser enters powder catcher with inert gas, then toward powder catcher
Interior gas-solid separator is filled with inert gas, focuses on the iron-nickel alloy of gas-solid separator outer wall higher than powder catcher bottom
Collection hopper in, realize gas solid separation, inert gas is recycled under the action of air-introduced machine.
2. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials according to claim 1, feature exist
In the mass ratio of: iron, nickel be 1:1-4；Iron, nickel can be pure metal mechanical mixture, be also possible to metal prefabricated in proportion
Block.
3. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials according to claim 1, feature exist
In: system pressure 50-120kPa.
4. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials according to claim 1, feature exist
In: the plasma gun in high-temperature evaporator is untransferable arc, and the working gas of plasma gun is nitrogen, hydrogen or ammonia etc..Deng
The power of ion gun is 60-100KW.
5. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials according to claim 1, feature exist
In: inert gas is nitrogen or argon gas.
6. a kind of submicron order iron-nickel alloy powder producing method of soft magnetic materials according to claim 1, feature exist
In: submicron order FeNi powders average grain diameter is 0.15-0.80 μm, and shape is ball-type.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110170659A (en) * | 2019-05-29 | 2019-08-27 | 宁波广新纳米材料有限公司 | The production method of ball-type nano-tungsten powder |
| CN110935885A (en) * | 2019-11-11 | 2020-03-31 | 山西中磁尚善科技有限公司 | Flaky metal grinding process |
| CN110947977A (en) * | 2019-11-22 | 2020-04-03 | 江苏博迁新材料股份有限公司 | Production method of submicron AgSnTe alloy powder |
| CN113967735A (en) * | 2021-10-20 | 2022-01-25 | 广东长信精密设备有限公司 | Metal powder mixing method |
| CN115401207A (en) * | 2022-07-23 | 2022-11-29 | 杭州新川新材料有限公司 | Apparatus for producing mixed metal powder |
| CN117497278A (en) * | 2023-12-29 | 2024-02-02 | 天通控股股份有限公司 | High-permeability low-loss iron-based amorphous composite magnetic powder core and preparation method thereof |
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| CN102950290A (en) * | 2012-10-15 | 2013-03-06 | 宁波广博纳米新材料股份有限公司 | Method for producing nanoscale nickel-manganese alloy powder |
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| CN113967735A (en) * | 2021-10-20 | 2022-01-25 | 广东长信精密设备有限公司 | Metal powder mixing method |
| CN115401207A (en) * | 2022-07-23 | 2022-11-29 | 杭州新川新材料有限公司 | Apparatus for producing mixed metal powder |
| CN117497278A (en) * | 2023-12-29 | 2024-02-02 | 天通控股股份有限公司 | High-permeability low-loss iron-based amorphous composite magnetic powder core and preparation method thereof |
| CN117497278B (en) * | 2023-12-29 | 2024-03-12 | 天通控股股份有限公司 | High-permeability low-loss iron-based amorphous composite magnetic powder core and preparation method thereof |
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Application publication date: 20190507 |