CN103447542B - A kind of preparation method of micron order iron-based hollow ball material and device thereof - Google Patents

Abstract

The present invention relates to a kind of preparation method of micron order iron-based hollow ball material, belong to new function Building Decoration Material technical field.The invention provides a kind of aerosolization legal system for metal hollow ball material, control certain nitrogen pressure, make the superheated melt atomization being dissolved with gas and having gas-forming property material be fine droplet.Atomized drop is under the quick cooling of atomizing medium, drip gauge kept man of a noblewoman first solidifies formation solidified shell, stop gas evolution drop surface, reduce the reduction of process gas solubility in drop temperature and dissolved gas is separated out, enter drop internal and form cavity, shrink because the change of liquid-solid volume makes droplet size reduce fast in process of setting simultaneously, impel formation hollow metal sphere.The present invention can produce larger micron even other hollow ball of grade, and sphericity is high, and particle size range is from several microns to hundreds of micron Normal Distribution, and because cooling velocity is fast, so organize more tiny, oxygen content is low, and hardness is higher.

Description

A kind of preparation method of micron order iron-based hollow ball material and device thereof

Technical field

The present invention relates to a kind of method preparing micron order material hollow ball, particularly relate to the method preparing iron-based micron order hollow ball material, belong to Building Decoration Material technical field.

Background technology

Tiny balloon belongs to how empty material, there is low-density, the characteristic of high-ratio surface and unique mechanics thermal property, it can not only improve the character of matrix material to make it in light material, have important application, also can give material new performance, as heat insulation in sound isolating and flame-retardant etc., therefore, hollow ball material has very large potential using value in fields such as Building Decoration Material coatings industries and hollow space can hold a large amount of guest molecule or large scale object, produce the character based on microcosmic " parcel " effect that some are peculiar, tiny balloon is made to have broad prospect of application as a kind of new function material.The making of current hollow ball has a lot of method, the method of comparative maturity has: template, microemulsion method, interface self-assembling reaction method, masterplate-interfacial reaction method, hydro-thermal solvent reaction method, spray-on process, supercritical ultrasonics technology and gamma-rays irradiation etc., preparation method, often kind of method has its pluses and minuses, main still based on template at present, but these technology all seldom carry out the preparation of high-melting-point iron hollow ball, and the bad control of technical sophistication, make simultaneously for nanometer or other hollow powder of micro/nano level on the high side, little research tens is to hundreds of micron level even other hollow powder of grade.

Summary of the invention

The object of this invention is to provide the method for a kind of aerosolization legal system for micron order iron-based hollow ball material.

The present invention is the preparation method of the iron-based hollow ball material of a kind of micron, it is characterized in that having following technical process and step:

A. be put in the crucible of induction melting room by pure iron and another kind of simple metal manganese or molybdenum or non-metal carbon according to certain ratio, the mass ratio of pure iron and another kind of simple metal or non-metal carbon is (80-98): (20-2);

B. adopt the conventional aerosolization system and device of tradition to be prepared, its each technological parameter is as follows:

The preheat temperature of crucible is: 1000 DEG C-1600 DEG C; Monitor system is 30kW; Controlling the degree of superheat is 200 DEG C-420 DEG C; During system melting, vacuum is within 10Pa; Atomization nitrogen pressure is 0.60-2.20MPa; It is 0.1-0.5MPa that nitrogen returns pressurising power.

The device that micron order iron-based hollow ball preparation method is used, it is the device of traditional common, includes melting power supply, holding furnace power supply, vacuum system, water-cooling system, cyclone separator, powder gathering system.It is characterized in that, gas atomization device used is provided with inductive crucible, insulation crucible, nozzle, atomization

District, and nozzle is circular seam type close-coupled nozzle, is provided with mozzle, it is characterized in that mozzle protrudes length is 3.2-9.5mm, through 3.0-6.5 mm in mozzle.

The present invention is to provide a kind of aerosolization legal system for iron-based hollow ball material, controls certain nitrogen pressure, makes the superheated melt atomization being dissolved with gas and having gas-forming property material be fine droplet.Atomized drop is under the quick cooling of atomizing medium, drip gauge kept man of a noblewoman first solidifies formation solidified shell, stop gas evolution drop surface, reduce the reduction of process gas solubility in drop temperature and dissolved gas is separated out, enter drop internal and form cavity, shrink because the change of liquid-solid volume makes droplet size reduce fast in process of setting simultaneously, impel formation hollow metal sphere.The invention solves the method preparing micron order iron-based hollow ball material, and simple to operate, production rate is high, and the sphericity of hollow ball is high, controlled, can large-scale production, and this technical method need not any chemical reagent simultaneously, catalyst, non-environmental-pollution.

The invention has the beneficial effects as follows the preparation can carrying out high-melting-point iron hollow ball, comprise ferrous magnetic material, the present invention can produce larger micron even other hollow ball of grade, sphericity is high, particle size range from several microns to hundreds of micron Normal Distribution, because cooling velocity is fast, so organize more tiny, oxygen content is low, and hardness is higher.

Accompanying drawing explanation

Fig. 1 is the aerosolization system and device schematic diagram that the present invention utilizes.

Fig. 2 is the hollow ball material metallograph of the different irons that the present invention prepares.(a) Fe-13Mn hollow ball material cross section metallograph (b) high molybdenum cast iron hollow ball material cross section metallograph (c) Fe-17Mn hollow ball material cross section metallograph (d) casting pig HT150 hollow ball material cross section metallograph.

Detailed description of the invention

Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.

embodiment 1

1. by pure iron and pure manganese (99.7%) 5kg, be put in the dry pot of induction melting room (Fig. 1) according to quality 87:13, it is 3.5-9.5mm that adjustment jet nozzle flow guide pipe protrudes length, internal diameter 3.0-5.5mm.

2. open electric cabinet power supply and source of the gas (Fig. 1), water-cooling system, hydraulic pressure is adjusted to 0.3-0.4MPa, opens holding furnace power supply and carries out preheating, preheat temperature 1100 DEG C-1550 DEG C to insulation crucible.

3. open melting power switch, adjustment hydraulic pressure, opens inverse switch, regulates intermediate frequency, makes its starting of oscillation, slower power is adjusted to 30kW.After treating alloy melting, control the degree of superheat 220 DEG C-420 DEG C (infrared measurement of temperature).During closedown, slowly turn down power, intermediate frequency is down to 0, close inversion, finally close melting power switch (Fig. 1).

4. nitrogen returns and fills, and returning pressurising power is 0.15-0.45MPa, sees after having liquid to flow out from refluence pipe, opens source of the gas rapidly, and control air pressure 0.65-2.15MPa, complete atomization.Atomization process terminates latter 5 minutes, closes water-cooled and power supply, collect powder after waiting powder to cool.

5. if Fig. 2 (a) is obtained Fe-13Mn hollow ball material.

embodiment 2

1. by pure iron and pure manganese 5kg, be put in the dry pot of induction melting room (Fig. 1) according to quality 83:17, it is 3.0-9.0mm that adjustment jet nozzle flow guide pipe protrudes length, internal diameter 3.5-5.5mm.

2. open electric cabinet power supply and source of the gas (Fig. 1), water-cooling system, hydraulic pressure is adjusted to 0.3-0.4MPa, opens holding furnace power supply and carries out preheating, preheat temperature 1150 DEG C-1550 DEG C to insulation crucible.

3. open melting power switch, adjustment hydraulic pressure, opens inverse switch, regulates intermediate frequency, makes its starting of oscillation, slower power is adjusted to 30kW.After treating alloy melting, control the degree of superheat 250 DEG C-420 DEG C (infrared measurement of temperature).During closedown, slowly turn down power, intermediate frequency is down to 0, close inversion, finally close melting power switch (Fig. 1).

4. nitrogen returns and fills, and returning pressurising power is 0.1-0.45MPa, sees after having liquid to flow out from refluence pipe, opens source of the gas rapidly, and control air pressure 0.65-2.05MPa, complete atomization.Atomization process terminates latter 5 minutes, closes water-cooled and power supply, collect powder after waiting powder to cool.

5. if Fig. 2 (c) is obtained Fe-17Mn hollow ball material.

embodiment 3

1. be put in by high molybdenum cast iron in the dry pot of induction melting room (Fig. 1), it is 3.2-9.0mm that adjustment jet nozzle flow guide pipe protrudes length, internal diameter 3.5-6.5mm.

2. open electric cabinet power supply and source of the gas (Fig. 1), vacuum, water-cooling system, hydraulic pressure is adjusted to 0.3-0.4MPa,

3. close all valves, when being evacuated within 10Pa, opening holding furnace power supply and preheating is carried out, preheat temperature 1150 DEG C-1450 DEG C to insulation crucible.

4. open melting power switch, adjustment hydraulic pressure, opens inverse switch, regulates intermediate frequency, makes its starting of oscillation, slower power is adjusted to 30kW.After treating alloy melting, control the degree of superheat 260 DEG C-400 DEG C (infrared measurement of temperature).During closedown, slowly turn down power, intermediate frequency is down to 0, close inversion, finally close melting power switch (Fig. 1).

5. nitrogen returns and fills, and returning pressurising power is 0.15-0.4MPa, sees after having liquid to flow out from refluence pipe, opens source of the gas rapidly, and control air pressure 0.63-2.00MPa, complete atomization.Atomization process terminates latter 5 minutes, continues to vacuumize equipment, closes water-cooled and power supply, collect powder after waiting powder to cool.

6. if Fig. 2 (b) is obtained high molybdenum cast iron hollow ball material.

embodiment 4

1. be put in by casting pig HT150 in the dry pot of induction melting room (Fig. 1), it is 3.2-8.5mm that adjustment jet nozzle flow guide pipe protrudes length, internal diameter 3.5-6.5mm.

2. open electric cabinet power supply and source of the gas (Fig. 1), vacuum, water-cooling system, hydraulic pressure is adjusted to 0.3-0.4MPa,

Close all valves, when being evacuated within 10Pa, opening holding furnace power supply and preheating is carried out, preheat temperature 1100 DEG C-1450 DEG C to insulation crucible.

3. open melting power switch, adjustment hydraulic pressure, opens inverse switch, regulates intermediate frequency, makes its starting of oscillation, slower power is adjusted to 30kW.After treating alloy melting, control the degree of superheat 310 DEG C-420 DEG C (infrared measurement of temperature).During closedown, slowly turn down power, intermediate frequency is down to 0, close inversion, finally close melting power switch (Fig. 1).

4. nitrogen returns and fills, and returning pressurising power is 0.2-0.45 MPa, sees after having liquid to flow out from refluence pipe, opens source of the gas rapidly, and control air pressure 0.83-2.20MPa, complete atomization.Atomization process terminates latter 5 minutes, continues to vacuumize equipment, closes water-cooled and power supply, collect powder after waiting powder to cool.

If Fig. 2 (d) is obtained casting pig HT150 hollow ball material.

Claims (1)

1. a preparation method for micron order iron-based hollow ball material, is characterized in that having following technical process and step:

A. be put in the crucible of induction melting room by pure iron and another kind of simple metal manganese or molybdenum or non-metal carbon according to certain ratio, the mass ratio of pure iron and another kind of simple metal or non-metal carbon is (80-98): (20-2);

B. adopt the conventional aerosolization system and device of tradition to be prepared, its each technological parameter is as follows:

The preheat temperature of crucible is: 1000 DEG C-1600 DEG C; Monitor system is 30kW; Controlling the degree of superheat is 200 DEG C-420 DEG C; During system melting, vacuum is within 10Pa; Atomization nitrogen pressure is 0.60-2.20MPa; It is 0.1-0.5MPa that nitrogen returns pressurising power.