CN107199347A - A kind of preparation method of superfine spherical iron powder - Google Patents
A kind of preparation method of superfine spherical iron powder Download PDFInfo
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- CN107199347A CN107199347A CN201710222507.5A CN201710222507A CN107199347A CN 107199347 A CN107199347 A CN 107199347A CN 201710222507 A CN201710222507 A CN 201710222507A CN 107199347 A CN107199347 A CN 107199347A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
A kind of preparation method of superfine spherical iron powder, a）By calcium oxide and croci in mass ratio 2~7:8~3 carry out ball milling mixing, the h of ball milling 4~6, with the powder being uniformly mixed；b）Uniform mixed powder is heated to 1100~1300 DEG C in air or oxygen atmosphere, 2~4 h is incubated, obtains calcium ferrite presoma；c）By step b）Obtained calcium ferrite is heated to 850~1000 DEG C in hydrogen atmosphere, is incubated 1~3 h, obtains the mixed-powder of calcium oxide and nanometer iron powder；d）It is that 0.2 mol/L ammonium chloride solutions clean reduzate repeatedly with concentration, is then cleaned repeatedly with deionized water and absolute ethyl alcohol, obtain wet iron powder；e）The wet iron powder of gained is put into 50 DEG C of 1~3 h of drying in vacuum drying chamber.Ferrous powder granules prepared by the present invention are tiny, epigranular；Production process iron powder is difficult to be oxidized；Technique is simple, with low cost, can serialization production in enormous quantities.
Description
Technical field
The present invention relates to a kind of preparation method of new superfine spherical iron powder.
Background technology
Superfine iron powder has larger specific surface area and surface-active because of it, anti-in electricity, magnetic, light, catalysis, absorption and chemistry
There is special performance so that its purposes is extremely wide in terms of answering, be generally used for powder metallurgy, manufacture machine components, life
In terms of production friction material, antifriction material, steel bonded carbide, magnetic material, lubricant, and in chemical industry, cutting, heating material
The fields such as material, welding rod, which also have, widely to be used.In recent years, with the continuous research and development to superfine iron powder so that ultra-fine iron
Powder also has broad application prospects in fields such as electromagnetism, biomedicine, optics, metallurgy.
Iron powder, as iron-base powder metallurgy material and the primary raw material of product, is one of consumption maximum in powder metallurgy industry
Class powder.With the rapid development of the national economy, the industry such as automobile, engineering machinery greatly develop brought to iron powder it is wide
Development prospect.At present, iron-base powder metallurgy material develops towards high density, high intensity, complex-shaped direction, to the technique of raw material
Performance proposes higher and higher requirement.But China's PRODUCTION OF IRON POWDER small scale, efficiency are low, batch is small, powder property stability
It is poor；Iron powder is of less types, and new varieties are inadequate；Iron powder product totally improves grade not high, many high-performance, complex-shaped zero
The production of part largely or entirely dependence on import, and basic data is imperfect so far.So that the basic research to iron powder shows
Obtain particularly important.
And at present all there is respective shortcoming in the production technology of domestic superfine iron powder：The iron particle size that carbonyl process is prepared point
Cloth is concentrated, though industrial production is realized, due to Fe (CO)5For poisonous explosive material, prepare and complex manufacturing and be difficult
Control, fairly large production can not be realized by causing；And the iron powder particle diameter that gas phase reduction process is prepared is small, size distribution is concentrated,
But reaction is gas phase reaction, process is fine, is difficult to control, it is difficult to realize industrialized production；And the physical method such as vaporization condensation process
Need to carry out under preferable vacuum condition, be difficult in actual industrial production.
The present invention prepares superfine spherical iron powder method, technique very simple, low for equipment requirements, low raw-material cost, production
Product purity height and epigranular.
The content of the invention
The purpose of the present invention is, for the deficiency in existing technology of preparing, to propose a kind of preparation of new superfine spherical iron powder
Method, nanometer iron powder is prepared by calcium ferrite hydrogen reduction, and technique is simple, with low cost, can obtain uniform superfine spherical iron
Powder.
The present invention is achieved by the following technical solutions：
The present invention is mixed using calcium oxide with iron oxide by proper proportion, and carries out spheroidal graphite batch mixing, then carries out calcining preparation forerunner
Body；Then presoma is reduced to the mixed-powder for obtaining CaO and Fe with hydrogen, is 0.2 mol/LNH using concentration4Cl solution is clear
Wash reduzate and can obtain superfine spherical iron powder.
A kind of preparation method of superfine spherical iron powder of the present invention, according to the following steps.
a）Batch mixing：By calcium oxide and croci in mass ratio 2~7:8~3 carry out ball milling mixing, and Ball-milling Time is 4
~6 h, with the powder being uniformly mixed.
b）Calcining：Uniform mixed powder is heated to 1100~1300 DEG C in air or oxygen atmosphere, insulation 2~
4 h, obtain calcium ferrite presoma.
c）Reduction：By step b）Obtained calcium ferrite is heated to 850~1000 DEG C in hydrogen atmosphere, is incubated 1~3 h,
Obtain the mixed-powder of calcium oxide and nanometer iron powder.
d）Cleaning：It is that 0.2 mol/L ammonium chloride solutions clean reduzate repeatedly with concentration, then with deionized water and nothing
Water-ethanol is cleaned repeatedly, obtains wet iron powder.
e）Dry：The wet iron powder of gained is put into 50 DEG C of 1~3 h of drying in vacuum drying chamber, superfine spherical iron is finally obtained
Powder.
It is an advantage of the invention that.
（1）The ferrous powder granules that the preparation method that the hydrogen reduction calcium ferrite that the present invention is provided prepares nanometer iron powder is obtained are tiny,
Epigranular.
（2）In the cleaning of whole reduzate and drying process, all iron powder is avoided directly to be contacted with air as far as possible so that iron
Powder is difficult to be oxidized.
（3）This method technique is simple, and with low cost, iron oxide and calcium oxide in raw material are the common raw material of industry,
Calcining and reduction process without particular/special requirement, are conducive to serialization to produce in enormous quantities equipment.
Brief description of the drawings
Fig. 1 is the SEM figures of the iron powder of the gained of embodiment 1.
Embodiment
The present invention will be described further by following examples, but protection scope of the present invention not limited to this.
Embodiment 1.
（1）By calcium oxide and croci in mass ratio 7:The 3 mixing h of spheroidal graphite 4, rotating speed is 120 rad/s.
（2）The mixed-powder obtained after spheroidal graphite is put into corundum boat, is placed in tube furnace, makes to forge in its air atmosphere
Burn, calcining heat is 1100 DEG C, is incubated 2 h, obtains calcium ferrite.
（3）It is placed in being put into after the powder mull after calcining in quartz boat in tube furnace, it is gone back in hydrogen atmosphere
Original, reduction temperature is 850 DEG C, is incubated 2 h, obtains the mixed-powder of calcium oxide and iron.
（4）The powder that reduction is obtained is put into 0.2 mol/L ammonium chloride solution, and is stirred continuously, and is cleaned 3 times repeatedly
After carry out separation of solid and liquid.
（5）Residual powder is cleaned 3 times with deionized water, then with washes of absolute alcohol wet-milling 3 times.Vacuum is finally putting into do
With 50 DEG C of dry 1 h in dry case, iron powder is obtained.
Embodiment 2.
（1）By calcium oxide and iron oxide in mass ratio 1:The h of 1 mixing and ball milling 4, rotational speed of ball-mill is 120 rad/s.
（2）Mixed-powder after ball milling is put into corundum boat, is placed in tube furnace, it is forged in air atmosphere
Burn, calcining heat is 1000 DEG C, is incubated 2 h, obtains calcium ferrite.
（3）It will be put into quartz boat, be placed in tube furnace after powder mull after calcining, it is gone back in hydrogen atmosphere
Original, reduction temperature is 800 DEG C, is incubated 2 h, obtains the mixed-powder of iron and calcium oxide.
（4）In the ammonium chloride solution that powder after carrying out reduction is put into 0.2 mol/L, it is stirred continuously, after cleaning 3 times repeatedly
Carry out separation of solid and liquid.
（5）Residual powder is cleaned 3 times with deionized water, then with washes of absolute alcohol wet-milling 3 times.Vacuum is finally putting into do
With 50 DEG C of dry 1 h in dry case, iron powder is obtained.
Claims (1)
1. a kind of preparation method of superfine spherical iron powder, it is characterized in that according to the following steps：
a）By calcium oxide and croci in mass ratio 2~7:8~3 carry out ball milling mixing, and Ball-milling Time is 4~6 h, with
To mixed uniformly powder；
b）Uniform mixed powder is heated to 1100~1300 DEG C in air or oxygen atmosphere, 2~4 h is incubated, obtains
Calcium ferrite presoma；
c）By step b）Obtained calcium ferrite is heated to 850~1000 DEG C in hydrogen atmosphere, is incubated 1~3 h, obtains calcium oxide
With the mixed-powder of nanometer iron powder；
d）It is that 0.2 mol/L ammonium chloride solutions clean reduzate repeatedly with concentration, it is then anti-with deionized water and absolute ethyl alcohol
Multiple cleaning, obtains wet iron powder；
e）The wet iron powder of gained is put into 50 DEG C of 1~3 h of drying in vacuum drying chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710222507.5A CN107199347A (en) | 2017-04-07 | 2017-04-07 | A kind of preparation method of superfine spherical iron powder |
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| CN201710222507.5A CN107199347A (en) | 2017-04-07 | 2017-04-07 | A kind of preparation method of superfine spherical iron powder |
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| Publication Number | Publication Date |
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| CN107199347A true CN107199347A (en) | 2017-09-26 |
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| CN201710222507.5A Pending CN107199347A (en) | 2017-04-07 | 2017-04-07 | A kind of preparation method of superfine spherical iron powder |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077694A (en) * | 2016-08-08 | 2016-11-09 | 南昌大学 | A kind of preparation method of spherical cobalt powder |
| CN106424751A (en) * | 2016-11-18 | 2017-02-22 | 南昌大学 | Preparation method of nano copper powder |
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2017
- 2017-04-07 CN CN201710222507.5A patent/CN107199347A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077694A (en) * | 2016-08-08 | 2016-11-09 | 南昌大学 | A kind of preparation method of spherical cobalt powder |
| CN106424751A (en) * | 2016-11-18 | 2017-02-22 | 南昌大学 | Preparation method of nano copper powder |
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Application publication date: 20170926 |