CN100488673C - Method of manufacturing micro and sub-micron iron powder - Google Patents
Method of manufacturing micro and sub-micron iron powder Download PDFInfo
- Publication number
- CN100488673C CN100488673C CNB2007100636322A CN200710063632A CN100488673C CN 100488673 C CN100488673 C CN 100488673C CN B2007100636322 A CNB2007100636322 A CN B2007100636322A CN 200710063632 A CN200710063632 A CN 200710063632A CN 100488673 C CN100488673 C CN 100488673C
- Authority
- CN
- China
- Prior art keywords
- iron powder
- gas
- volume content
- passivation
- nitrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 64
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 45
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000002161 passivation Methods 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000003595 mist Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 239000002184 metal Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- 230000000415 inactivating effect Effects 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 25
- 235000013980 iron oxide Nutrition 0.000 description 16
- 229910052742 iron Inorganic materials 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000036632 reaction speed Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229940067573 brown iron oxide Drugs 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000000713 high-energy ball milling Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- IGHXQFUXKMLEAW-UHFFFAOYSA-N iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Fe+2].[O-2] IGHXQFUXKMLEAW-UHFFFAOYSA-N 0.000 description 1
- 238000001725 laser pyrolysis Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to the making of micron and sub-micron metal powder, which firstly ball grinds the oxidized metal powder with heating environment, entering nitrogen or argon gas or their mixture till the content of metal powder <=10 micron, heating it to 200-400deg.C, feeding recovery gas H2 or mixture of H2 and CO to switch nitrogen and argon or their mixture for 30-6000 min, removing the water and CO2, boosting to back to the ball grinding for reaction, inactivating the recovered iron powder. It is low in cost and energy consumption, simple in production process, easy in making, suitable for mass production.
Description
Technical field
The invention belongs to field of powder metallurgy preparation, particularly the preparation method of micron order, submicron order iron powder.
Background technology
In the prior art, micron order, submicron order iron powder are one of basic materials of powder metallurgy industry, and the granularity of micron order iron powder is that 1～10 micron, the granularity of submicron order iron powder are 0.1～1 micron.Micron order, submicron order iron powder have bigger specific area and activity, be mainly used in powder metallurgy, manufacturing machine part, produce fields such as friction material, antifriction material, superhard material, magnetic material, lubricant and goods thereof, in recent years, still have broad application prospects at numerous areas such as electromagnetism, biology, medical science, optics.
Tradition iron powder major part is by reducing process production.Reducing process mainly uses gas base or the coal-based pure iron oxide raw material that at high temperature reduces to obtain iron powder.Because the reduction temperature height, the granularity of iron powder is bigger, is difficult to prepare micron order, submicron order iron powder.In addition, atomization also can the production granularity iron powder suitable with reducing process.In order to prepare micron order, submicron order iron powder, adopt following several method usually:
(1) gas phase reduction process
Gas phase reduction process generally is with FeCl
2At high temperature evaporate in molysite, in gas phase, use H
2Or NH
3Make reducing agent and prepare superfine iron powder.Course of reaction is divided into molysite dehydration, evaporation and three steps of vapour phase reduction.α in the gas phase reduction process
FeMoment nucleation, nucleation temperature is lower, the iron powder particle diameter is little, size distribution is concentrated; But because of it reacts when the gas phase, course of reaction is meticulous, is subjected to the influence of device etc. easily, and stability is bad, has not yet to see production in enormous quantities.
(2) solid phase reduction method
The solid phase reduction method generally refers at H
2Under the atmosphere, with FeC
2O
42H
2Presoma such as O or FeOOH decomposes, reduction is with the preparation superfine iron powder, reduction temperature 510 ℃ proper, this method requires high to the preparation of presoma, also be difficult at present make on a large scale.
(3) carbonyl process
The preparation method of carbonyl iron dust is generally the ordinary hot decomposition method, promptly allows Fe (CO)
5Directly decompose at a certain temperature and produce iron powder.The laser pyrolysis ratio juris is to utilize the continuous laser current system, with carbonyls Fe (CO)
5Cracking prepares superfine iron powder.But because the carbonyl process system cost is higher, and Fe (CO)
5Be poisonous explosive material, the complicated operation of whole process flow, these have hindered the application popularization of carbonyl process.
(4) vacuum vapor deposition method and sputtering method
Vacuum vapor deposition method is meant and makes evaporation of metal in a vacuum, then with its steam cooling with condense, and obtains the method for ultrafine metal powders.Sputtering method is to utilize sputtering phenomenon to replace evaporation to prepare dystectic super-fine metal powder, can be used for the preparation of metal iron powder.The advantage of these class methods is that the superfine powder size distribution of preparation is concentrated, uniform particles, and vacuum environment was difficult to realize when shortcoming was industrial production.
(5) high-energy ball milling method
High-energy ball milling method is rotation or the vibration that utilizes ball mill, makes hard sphere carry out strong bump, mill and stir metallic iron, powder is pulverized be the method for ultrafine dust.Because metallic iron has cold draw, the preparation micron order, submicron order iron powder difficulty is big, energy consumption is high.
Summary of the invention
The object of the present invention is to provide that a kind of cost is low, energy consumption is low, production process is simple to operate, easy preparation, be applicable to production in enormous quantities, the micron order that the iron powder reducing rate is high, the preparation method of submicron order iron powder.
According to above-mentioned purpose, the principle of the inventive method is:
The preparation method of the micron order that we proposed, submicron order iron powder mainly designs at the deficiency in the existing technology of preparing, for example, High Temperature Gas base and coal base reduction method reduction temperature height, iron particle size is big; High-energy ball milling method is because the distinctive ductility of iron powder is milled down to micron order or submicron order is quite difficult, and power consumption is high.The preparation method of micron order proposed by the invention, submicron order iron powder combines the advantage of gas base reducing process and ball-milling method, and iron oxide belongs to brittle substance, and iron powder belongs to ductile material, so easier micron order or the submicron order of being crushed to of iron oxide.In the iron oxide thinning process, mechanical energy partly is converted into surface energy, crystal boundary energy and the distortion of lattice energy etc. of ferric oxide powder, realizes the energy storage of ferric oxide powder.According to thermodynamics of reactions and dynamic law, the fine powder body of energy storage helps the reduction of reaction temperature, the quickening of reaction speed.Experiment according to us can be reduced to the reaction temperature of the thin iron oxide of gas reduction below 500 ℃, far below the reduction temperature of coal-based method or traditional gas base method.From H
2Reduction Fe
2O
3Thermodynamical equilibrium figure (Fig. 1) as can be known, when temperature was lower than 200 ℃, the utilization rate of hydrogen extremely low (being lower than 1%) was though H in theory
2Still can reducing iron oxides, but efficient is very low, has not had productive value.Therefore, the temperature in the ball mill should be controlled at more than 200 ℃.But too high temperature is too high to device, the material requirement of ball mill, and according to our research, it is relatively more suitable that the temperature in the ball mill is controlled at 200～400 ℃.
CO also is a reducibility gas preferably, and from the thermodynamical equilibrium figure (Fig. 2) of CO reducing iron oxides as seen, under equilibrium condition, CO compares H
2The utilization rate height, but the reaction speed of CO is lower than H under the low temperature
2, CO analyses the trend of carbon in addition under the low temperature simultaneously, hinders the carrying out of reaction.According to our result of study, the volume content percentage of CO is advisable to be lower than 30%.
Because reduction temperature is lower, the utilization rate of gas is still not high, and this meaning is left in the tail gas of ball mill except product H
2O and CO
2Still there are a large amount of H outward,
2, CO.If directly be discharged in the atmosphere, not only cause the waste of the energy, the more important thing is the production cost that has increased iron powder.Therefore, the present invention has designed the H that removes earlier in the tail gas
2O and CO
2, reducibility gas is reused through after the supercharging then.
The reducibility gas that the present invention uses is with H
2, CO is main, but steam, carbon dioxide, oxygen etc. had strict demand, because the carrying out that these gases hinder reduction reaction.According to our experiment, the volume content of steam should be less than 1% in the reducibility gas, and the volume content of oxygen should be less than 0.5%, CO
2Volume content should be less than 5%.Though gas such as nitrogen, argon gas does not participate in reduction reaction, they can dilute the concentration of reducibility gas, and then influence reaction speed, so their volume content is to be advisable less than 30%.
Ball mill apparatus in the actual fabrication process comprises agitating ball mill, vibrator and planetary mills etc.In order to satisfy the requirement of reduction temperature, need these devices are added heating function, can satisfy requirement of the present invention.
Circularly-supercharged equipment, as circulating pump, compressor and air blast series etc., these equipment in the market can satisfy supercharging requirement of the present invention.
According to above-mentioned purpose and method principle, concrete technical scheme of the present invention comprises following concrete steps:
A, pure raw iron oxide material powder put into the ball mill with heating function carry out ball milling, feed nitrogen or argon gas or its two mist simultaneously, until the croci granularity reach≤10 microns;
B, the ball milling built-in temperature is risen to 200-400 ℃, feed reducing gas H simultaneously
2Or H
2Reduce after switching nitrogen or argon gas or its two mist with the CO mist, the time is 30-600min;
C, the tail gas that will reduce are removed water and CO
2After utilize supercharger to feed again to participate in reaction in the ball mill;
D, the iron powder that reduces is carried out Passivation Treatment.The idiographic flow of this Passivation Treatment is to fill in the ball mill of superfine iron powder containing a certain amount of passivation gas feeding; utilize passivation gas and/or nitrogen, water quench means earlier the temperature of high temperature superfine iron powder to be reduced between room temperature～200 ℃; and then logical passivation gas and keep 30min～600min; make the surface of superfine iron powder form one deck protective oxide film; thereby reach the iron powder passivation effect, CO in the used passivation gas in the said method
2Volume content is 50-100%, and the M volume content is 0-50%, and wherein M is any one or any one the above volume content sum in oxygen, CO, steam, nitrogen or the argon gas.
In addition, guarantee atmosphere percentage in the ball mill: volume content percentage≤1% of steam, volume content percentage≤0.5% of oxygen, CO
2Volume content percentage≤5%, volume content percentage≤30% of nitrogen and argon gas, CO volume content percentage＜30%, all the other are gas H
2
The 3rd, the volume content of oxygen≤5% in the passivation gas, CO and CO
2The ratio of volume content be 0～0.8, the volume content of steam≤5%, remaining gas do not participate in nitrogen, the argon gas of passivation reaction, its volume content is≤30%.
The present invention has compared with prior art that cost is low, energy consumption is low, production process is simple to operate, easy preparation, be applicable to production in enormous quantities, the advantage that the iron powder reducing rate is high.The percent reduction of the iron powder that is obtained 〉=98%.
In addition, the present invention compared with prior art has good passivation effect, sample and does not have that peroxidating, secondary oxidation rate are lower, the high advantage of degree of metalization of iron powder after the passivation.The advantage of this method is particularly in comparatively apace the surface oxidation of superfine iron powder being become Fe
3O
4Diaphragm, and needn't worry the peroxidating problem, and superfine iron powder is lower because of the secondary oxidation rate that passivation causes.
Description of drawings
Fig. 1 is the thermodynamical equilibrium figure of hydrogen reducing iron oxide.
Fig. 2 is the thermodynamical equilibrium figure of CO reducing iron oxides.
Fig. 3 obtains the shape appearance figure of trickle iron powder for adopting preparation method of the present invention.
The specific embodiment
The enforcement of the inventive method is earlier analytically pure brown iron oxide to be placed in the agitating ball mill with heating function, feeds nitrogen or argon gas the air in the ball mill is caught up with to the greatest extent.The starting agitating ball mill is milled down to brown iron oxide below 10 microns, and the ball milling built-in temperature is risen to 200～400 ℃.Switch nitrogen or argon gas with reducibility gas, begin to reduce, the tail gas that leaves ball mill removes H
2O/CO
2After, after the supercharging of coal gas supercharger, reuse.In the experimentation, hydrogen, CO, CO
2, nitrogen, argon gas, oxygen uses is 99.99% pure gas of commodity production, obtains steam by the steam generator, gas componant is regulated by the multipath gas control system, and uses the variation of online gas analyzer dynamic monitoring gas content.After the iron powder cooling after the reduction, the logical CO that contains
2Passivation gas iron powder is carried out passivation, implementation condition and result of implementation are all listed table 2 (experiment numbers 9～16) in.Except that passivation gas composition and passivation temperature are the variable, each heat of other experiment condition all is consistent, and contains CO
2Passivation gas prepare in advance, passivation time obtains by trial and error method, for example, as the passivation time deficiency, secondary oxidation will soon take place in the iron powder that takes out in air, should prolong passivation time this moment, secondary oxidation can not take place up to the iron powder that takes out in air, analyzes powder composition and pattern then.The inventive method prepares the implementation condition and the result of implementation of micron order, submicron order iron powder and all lists table 1 (experiment numbers 1～8) in.Table 3 is implemented and the comparison that has method now for the inventive method.
Prove that by the embodiment of the invention it is fully feasible using the inventive method production micron order, submicron order iron powder, the reducing rate of iron powder is very high, and the percent reduction of each heat has all surpassed 98%, and the part heat is up to more than 99.5%.
From embodiment as seen, along with the raising of reduction temperature, reaction speed is accelerated, corresponding shortening of reaction time.Because too high temperature is very high to device, the material requirement of ball mill, according to our research, it is relatively more suitable that the temperature in the ball mill is controlled at 200～400 ℃.
Though CO also can reducing iron oxides, find that in an embodiment CO content improves, the recovery time is elongated, this with low temperature under CO to analyse carbon relevant, therefore, it is more suitable that the volume content of CO is controlled at below 30%.
Oxygen, water vapour and carbon dioxide are unfavorable for the carrying out of reduction reaction, can prolong the recovery time.For carrying out smoothly of reduction reaction, the volume content of steam is less than 1% in the reducibility gas, and the volume content of oxygen is less than 0.5%, CO
2Volume content less than 5%.
Though nitrogen, argon gas do not participate in reduction reaction, can diluting reaction substrate concentration, thereby delayed response carry out, the production cycle is prolonged, their volume total content should be lower than 30%.
Table 1 the inventive method prepares the experiment condition and the result of micron order, submicron order iron powder
Table 2 contains CO
2The experiment condition and the result of gas passivation superfine iron powder
Table 3 the inventive method is implemented and the comparison that has method now
| Tradition gas base method | Coal-based method | Atomization | Carbonyl process | The present invention | |
| The major technique characteristics | Logical hydrogen reducing pure iron oxide under the high temperature (as iron scale etc.) | High temperature uses smart down.Coal reduction pure iron oxide | In the atomising device of atmosphere protection, molten steel is atomized | Iron pentacarbonyl is produced superfines through thermal decomposition | The pure brown iron oxide of reduction in having the efficient ball mill of heating function |
| Smelting temperature | 700～900 |
1000～1200 ℃ | 1600～1800 ℃ | 150～350 |
200～400 ℃ |
| Product purity | High | Low | High | High | High |
| Product granularity | Tens of microns | Tens of microns | Tens of microns | Several microns even thinner | Several microns even thinner |
| Raw material sources | Pure iron oxide, wide material sources, cost is low | Pure iron oxide, wide material sources, cost is low | Pure iron, wide material sources, cost is higher than pure iron oxide | Iron pentacarbonyl, preparation is complicated, and severe toxicity is arranged, and is with high costs | Pure iron oxide, wide material sources, cost is low |
| Capital equipment | Fluid bed | Tunnel cave | Vacuum smelting furnace, atomising device | The preparation equipment of iron pentacarbonyl, the iron pentacarbonyl pyrolysis device | Efficient ball mill with heating function |
| Production cost | Low | Low | Higher | Very high | Low |
Claims (2)
1, the preparation method of a kind of micron order, submicron order iron powder is characterized in that this preparation method comprises following concrete steps:
A, pure raw iron oxide material powder put into the ball mill with heating function carry out ball milling, feed nitrogen or argon gas or its two mist simultaneously, until the croci granularity reach≤10 microns;
B, the ball milling built-in temperature is risen to 200-400 ℃, feed reducing gas H simultaneously
2Or H
2Reduce after switching nitrogen or argon gas or its two mist with the CO mist, the time is 30-600min;
C, the tail gas that will reduce are removed water and CO
2After utilize supercharger to feed again to participate in reaction in the ball mill;
D, the superfine iron powder that reduces is carried out Passivation Treatment, the idiographic flow of this Passivation Treatment is to contain a certain amount of CO
2Passivation gas feed and to fill in the ball mill of superfine iron powder; utilize passivation gas and/or nitrogen, water quench means earlier the temperature of high temperature superfine iron powder to be reduced between room temperature～200 ℃; and then logical passivation gas and keep 30min～600min; make the surface of superfine iron powder form one deck protective oxide film; thereby reach the superfine iron powder passivation effect, CO in the used passivation gas in the said method
2Volume content is 50-100%, and the M volume content is 0-50%, and wherein M is any one or any one the above mixture in oxygen, CO, steam, nitrogen or the argon gas.
2, the preparation method of micron order according to claim 1, submicron order iron powder is characterized in that guaranteeing having atmosphere percentage in the ball mill of heating function: volume content percentage≤1% of steam, volume content percentage≤0.5% of oxygen, CO
2Volume content percentage≤5%, volume content percentage≤30% of nitrogen or argon gas or its two mist, volume content percentage＜30% of CO, all the other are H
2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100636322A CN100488673C (en) | 2007-02-07 | 2007-02-07 | Method of manufacturing micro and sub-micron iron powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100636322A CN100488673C (en) | 2007-02-07 | 2007-02-07 | Method of manufacturing micro and sub-micron iron powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101011746A CN101011746A (en) | 2007-08-08 |
| CN100488673C true CN100488673C (en) | 2009-05-20 |
Family
ID=38699566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100636322A Expired - Fee Related CN100488673C (en) | 2007-02-07 | 2007-02-07 | Method of manufacturing micro and sub-micron iron powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100488673C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880857B (en) * | 2010-06-10 | 2012-03-14 | 沈阳工业大学 | Direct-current arc method for preparing Al nano tadpoles |
| CN102139375A (en) * | 2011-03-18 | 2011-08-03 | 上海大学 | Method for preparing micron-size superfine iron powder |
| CN102756130A (en) * | 2012-07-11 | 2012-10-31 | 沈阳理工大学 | Preparation method of metal powder |
| CN103817340A (en) * | 2014-03-13 | 2014-05-28 | 抚顺龙诚新科技材料有限公司 | Preparation method for superfine pre-alloyed powder |
| CN104493192A (en) * | 2014-12-17 | 2015-04-08 | 上海寰保渣业处置有限公司 | Micron-sized ultrafine iron powder preparation method |
| CN104972134B (en) * | 2015-08-05 | 2017-02-01 | 河南聚鑫超硬材料有限公司 | Method for producing superfine iron powder |
| CN107971501B (en) * | 2017-11-29 | 2020-06-05 | 江西理工大学 | Method for preparing superfine copper powder by secondary atmosphere reduction |
| CN113118450B (en) * | 2019-12-31 | 2023-05-30 | 拓米(成都)应用技术研究院有限公司 | Preparation method of nano-scale and submicron-scale metal powder |
| CN113173604A (en) * | 2020-08-05 | 2021-07-27 | 河南济源钢铁(集团)有限公司 | Method for preparing nano iron and oxide thereof by taking sintering ash as raw material |
| CN113427013B (en) * | 2021-06-07 | 2022-11-08 | 中国恩菲工程技术有限公司 | Preparation method of copper-based aluminum oxide nano material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154608A (en) * | 1978-07-19 | 1979-05-15 | Uop Inc. | Production of high purity iron powder |
| CN1231223A (en) * | 1998-04-09 | 1999-10-13 | 丛文华 | Process for preparation of high-purity iron powder |
| CN1410552A (en) * | 2002-11-25 | 2003-04-16 | 莱芜钢铁集团粉末冶金有限公司 | Low apparent density reduction iron powder and its manufacturing method |
| US6569220B1 (en) * | 1995-12-13 | 2003-05-27 | Donald W. Clark | Iron powder and method of producing such |
| CN1480539A (en) * | 2002-09-04 | 2004-03-10 | 雨 赵 | Method for preparing ferrous powder by using coke oven gas to deoxidize powder of iron ore |
-
2007
- 2007-02-07 CN CNB2007100636322A patent/CN100488673C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154608A (en) * | 1978-07-19 | 1979-05-15 | Uop Inc. | Production of high purity iron powder |
| US6569220B1 (en) * | 1995-12-13 | 2003-05-27 | Donald W. Clark | Iron powder and method of producing such |
| CN1231223A (en) * | 1998-04-09 | 1999-10-13 | 丛文华 | Process for preparation of high-purity iron powder |
| CN1480539A (en) * | 2002-09-04 | 2004-03-10 | 雨 赵 | Method for preparing ferrous powder by using coke oven gas to deoxidize powder of iron ore |
| CN1410552A (en) * | 2002-11-25 | 2003-04-16 | 莱芜钢铁集团粉末冶金有限公司 | Low apparent density reduction iron powder and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101011746A (en) | 2007-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100488673C (en) | Method of manufacturing micro and sub-micron iron powder | |
| CN108080649B (en) | Method for preparing superfine iron powder by low-temperature hydrocarbon duplex reduction | |
| CN102974456B (en) | Separation process of refractory iron ore | |
| Hu et al. | Refined microstructure and enhanced mechanical properties in Mo-Y2O3 alloys prepared by freeze-drying method and subsequent low temperature sintering | |
| CN100444997C (en) | Simple fast preparing process of superfine WC-Co composite powder | |
| CN104988451B (en) | A kind of preparation method of ultrafine tungsten carbide base ball shaped thermal spray coating powder | |
| CN104801721A (en) | Equipment and method for preparing nanometer metal powder | |
| Tang et al. | Prospects of green extraction of iron from waste dumped flotation tailings by H2: A pilot case study | |
| CN103924111A (en) | Preparation method of hard alloy nanoparticle powder and high-performance sintered block material | |
| US20120328467A1 (en) | Method for the production of mixed oxides and permanent magnetic particles | |
| CN111968821A (en) | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof | |
| Ünal et al. | Direct reduction of ferrous oxides to form an iron-rich alternative charge material | |
| Gurmen et al. | Synthesis of nano-crystalline spherical cobalt–iron (Co–Fe) alloy particles by ultrasonic spray pyrolysis and hydrogen reduction | |
| CN103537688A (en) | Method for preparing Fe-Al alloy by using nano-powder | |
| JP2013204075A (en) | Method for producing fine reduced iron powder | |
| Zeng et al. | Influence of SiO2 on the gas-based direct reduction behavior of Hongge vanadium titanomagnetite pellet by hydrogen-rich gases | |
| CN103817340A (en) | Preparation method for superfine pre-alloyed powder | |
| Picas et al. | Nanocrystalline NiCrAlY powder synthesis by mechanical cryomilling | |
| CN111872414B (en) | Preparation method of micro-nano pre-alloyed powder | |
| CN101787406A (en) | Technology and device for non-smelting reduction of ultra-fine hematite powder | |
| CN108405874B (en) | A kind of preparation method of micron-size spherical iron powder | |
| CN109136788B (en) | High-carbon high-alloy amorphous pre-alloy powder and preparation method thereof | |
| CN110773750A (en) | Method and device for preparing high-purity superfine metal powder | |
| CN104308170A (en) | Superfine iron powder preparation method | |
| Sadykhov et al. | Development of a new combined process for nickel and cobalt recovery from ferriferous laterite ores |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090520 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |