CN103817340A - Preparation method for superfine pre-alloyed powder - Google Patents
Preparation method for superfine pre-alloyed powder Download PDFInfo
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- CN103817340A CN103817340A CN201310723092.1A CN201310723092A CN103817340A CN 103817340 A CN103817340 A CN 103817340A CN 201310723092 A CN201310723092 A CN 201310723092A CN 103817340 A CN103817340 A CN 103817340A
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Abstract
The invention belongs to the field of powered metallurgy powder manufacturing, and particularly relates to a method for directly passivating superfine metallurgy powder on a hydrogen reduction production line. The method specifically includes that A, a passivating section is continuously connected behind a cooling section on a common tubular hydrogen reduction furnace, wherein the passivating section is free of a heating or cooling device and with the length 1/2-4/5 of that of the reduction section; B, three passivation gas inlets are formed in the passivating section and are respectively located at the forefront and positions of 1/4 and 3/5 of the passivating section; C, passivation gas is air or oxygen and is led into the passivation gas inlets according to 0.1%-1% of reduced gas flow; D, a diffusion port with a valve is opened in the tail of the passivating section, and diffused gas flow is regulated to be 1/5-1/3 of that of the reduced gas flow; E, an automatic discharging box is received at the tail end of the passivating section with 60-degree slant angle. Compared with the prior art, the preparation method has the advantages of low investment, low cost, wide application, simplicity in production process and applicability to mass production.
Description
Technical field
The invention belongs to powder metallurgy powder and manufacture field, particularly a kind of preparation method of ultra-fine prealloy powder.
Background technology
Ultra-fine prealloy powder be a kind of particle diameter below 10 μ m, formed by two or more element, in the manufacture process of powder, alloying occurs, and all particles keep the metal dust of the component consistent with nominal content.Ultra-fine prealloy powder has the advantages such as active high, even tissue, fusing point are low, easy-sintering, has been subject to the great attention of Powder Metallurgy Industry, and has been widely used in diamond tool manufacture field.Ultra-fine iron nickel powder, iron ambrose alloy powder, iron cobalt copper powder, owing to diamond being had to good wetting and adhesive property, are used to manufacture Diamond Tool Matrix; Ultra-fine FeNi30 alloyed powder is during as the catalyst of diamond synthesis, has the advantages such as per unit area yield is high, material consumption is few, synthetic crystal mass is good.
At present, although a lot of for the manufacture of the method report of super fine pre-alloyed powder, what can be used in preparation of industrialization mainly contains three kinds of coprecipitation and atomization and mechanical alloying methods.
Coprecipitation is to add precipitating reagent in the solution that contains two or more metal ions, each metal ion species is precipitated simultaneously and obtain the uniform sediment of composition, then obtaining the method for alloy powder through operations such as thermal decomposition, reduction, fragmentation, screenings.The alloyed powder that the method is produced has fine size, particle size distribution is narrow, composition is even, purity is high, sintering activity advantages of higher, but maximum deficiency is that technique is too complicated, processing cost is high.
Atomization is the method that adopts high-pressure spray to smash motlten metal and then be cooled to powder particle.Although the method flow process alloyed powder composition short, that produce is even, obtain superfines to the requirement of equipment is very high, energy consumption is huge, processing cost is higher.
Mechanical alloying method, conventionally also referred to as high-energy ball milling method, is under protective atmosphere, and two or more metal dust by extruding, cold welding and pulverizing repeatedly, is realized alloying, thereby made ultra-fine prealloy powder in ball mill under solid-state.The method process is simple, but the time is long, production efficiency is extremely low, and extruding repeatedly makes that powder is inner produces very large internal stress, affects suppression performance and the sintering character of powder.
Summary of the invention
The invention provides that a kind of equipment investment is little, cost is low, energy consumption is low, production process is simple to operate, efficiency is high, be applicable to the preparation method of a kind of ultra-fine prealloy powder of producing in enormous quantities.
In order to realize foregoing invention object, technical scheme of the present invention is:
Metal oxide belongs to brittle substance, and metal dust belongs to ductile material, and therefore metal oxide is more easily crushed to micron order or submicron order.In metal oxide thinning process, mechanical energy Partial Conversion is surface energy, crystal boundary energy and the distortion of lattice energy etc. of oxide powder, this is not only conducive to the exchange of material between different metal oxides and compound, and the reduction temperature of metal oxide is significantly reduced.Take iron oxide as example, normal hydrogen reducing temperature is more than 900 ℃, and in the time being milled to 3 microns of granularity <, reduction temperature can be reduced to 380 ℃.Just, because fully levigate metal oxide can be at low temperature by hydrogen reduction, just guarantee that powder particle granularity in During Hydrogen Reducing is not grown up or the youthful and the elderly is large, for preparation superfines provides possibility.
Submicron metal has very high activity, in the time touching air, can be oxidized rapidly even spontaneous combustion, therefore must carry out Passivation Treatment.Passivation generally adopts containing micro-O
2inert gas, make superfines surface form protective oxide-film.This needs special paralysis facility and a large amount of inert gases.The present invention adopts the online passivating technique of tubular reduction furnace, is to add one section of passivation section at the afterbody of common tubular reduction furnace, micro-air or oxygen is directly passed into passivation section and realize online passivation.Air or oxygen because tube furnace internal gas pressure is for just, and have a small amount of reducing gases to flow to the discharge of stove tail, so can not flow to reduction section through cooling section.Our test has also confirmed this point.The in the situation that of definite in the recovery time, passivation time is decided by the length of passivation section.
According to above-mentioned purpose and Method And Principle, concrete technical scheme of the present invention comprises following concrete steps:
A, the metal oxides such as pure iron oxide, nickel protoxide put into high energy ball mill in proportion carry out ball milling, until oxide granularity reach≤3 microns.
B, the powder after ball milling is carried out in tube furnace to hydrogen reduction.Reducing gas is H
2or decomposed ammonia, reduction temperature are that 400 ~ 600 ℃, recovery time are 100 ~ 200min.
C, the alloyed powder reducing is carried out to Passivation Treatment.Passivation is carried out online in tube furnace: first at tube furnace cooling section, prealloy powder temperature is down to room temperature, then passes into micro-passivating gas in passivation section and make ultra-fine prealloy powder surface form protective oxide-film, thereby reach passivation effect.Passivating gas is air or O
2.
D, pulverizing.Powder after coming out of the stove has slightly bonding, breaks up with Ordinary pulverization machine.
E, screening.
F, finished product packing.
the invention has the beneficial effects as follows:
(1) the present invention compared with prior art has that equipment investment is little, cost is low, energy consumption is low, production process is simple to operate, efficiency is high, be applicable to the advantages such as production in enormous quantities.
(2) the present invention adopts the online passivating technique of tubular reduction furnace to save paralysis facility investment, has simplified production process operation, has saved the consumption of inert gas.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Fig. 2 is the tubular reduction furnace schematic diagram that has increased passivation section.
In figure, 1 is burner diffusion mouth; 2 is reduction section; 3 is reducing gases entrance; 4 is cooling section; 5 is passivating gas entrance; 6 is passivation section; 7 is stove tail diffusion mouth; 8 is discharging section.
Fig. 3 adopts preparation method of the present invention to obtain the shape appearance figure of ultra-fine FeNi powders.
The specific embodiment
The present invention for the preparation of the technological process of ultra-fine prealloy powder is: get the raw materials ready---ball milling---
---cooling---passivation---is pulverized---screening---finished product packing in hydrogen reduction.
Embodiment 1
Preparation FeNi25Cu5 prealloy powder
(1) get the raw materials ready: calculate and take various metal oxides by alloy requirement.Wherein, ferriferous oxide is electron level Fe2O3, and nickel oxide is electron level NiO, and Cu oxide is industrial one-level CuO.Below no longer explanation.
(2) ball milling: time 8h.
(3) hydrogen reduction: 600 ℃ of temperature, time 180min, reducing gases is decomposed ammonia (lower same).
(4) cooling: water-cooling jacket is forced cooling 60min.
(5) passivation: air mass flow is 0.3% of decomposed ammonia flow, passivation time 60min.
(6) pulverize: make quick beater by oneself.
(7) screening :-200 orders.
(8) packing: vacuum packaging.
Preparation FeCo25Cu25 prealloy powder
(1) get the raw materials ready: calculate and take various metal oxides by alloy requirement.Cobalt oxide is Y1 level.
(2) ball milling: time 10h.
(3) hydrogen reduction: 550 ℃ of temperature, time 120min.
(4) cooling: water-cooling jacket is forced cooling 60min.
(5) passivation: air mass flow is 0.2% of decomposed ammonia flow, passivation time 80min.
(6) pulverize: make quick beater by oneself.
(7) screening :-200 orders.
(8) packing: vacuum packaging.
Embodiment 3
Preparation FeNi30 prealloy powder
(1) get the raw materials ready: calculate and take various metal oxides by alloy requirement.
(2) ball milling: time 6h.
(3) hydrogen reduction: 650 ℃ of temperature, time 240min.
(4) cooling: water-cooling jacket is forced cooling 60min.
(5) passivation: air mass flow is 0.5% of decomposed ammonia flow, passivation time 30min.
(6) pulverize: make quick beater by oneself.
(7) screening :-200 orders.
(8) packing: vacuum packaging.
Claims (2)
1. a preparation method for ultra-fine prealloy powder, is characterized in that: this preparation method comprises following concrete steps:
A, the metal oxides such as pure iron oxide, nickel protoxide put into high energy ball mill in proportion carry out ball milling, until oxide granularity reach≤3 microns;
B, the powder after ball milling is carried out in tube furnace to hydrogen reduction, reducing gas is H
2or decomposed ammonia, reduction temperature are that 400 ~ 600 ℃, recovery time are 100 ~ 200min;
C, the alloyed powder reducing is carried out to Passivation Treatment;
?d, pulverizing, the powder after coming out of the stove has slightly bonding, breaks up with Ordinary pulverization machine;
E, screening;
F, finished product packing.
2. the preparation method of ultra-fine prealloy powder according to claim 1; it is characterized in that: passivation is carried out online in tube furnace: first at tube furnace cooling section, prealloy powder temperature is down to room temperature; then passing into micro-passivating gas in passivation section makes ultra-fine prealloy powder surface form protective oxide-film; thereby reach passivation effect; in whole cooling and passivating process, reducing gas is uninterrupted, and passivating gas is air or O
2.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104128613A (en) * | 2014-08-20 | 2014-11-05 | 丹阳市德源精密工具有限公司 | Preparation method for pre-alloyed powder |
| CN105345020A (en) * | 2015-11-15 | 2016-02-24 | 丹阳市德源精密工具有限公司 | Preparation method for pre-alloyed powder |
| CN109702217A (en) * | 2019-03-04 | 2019-05-03 | 江苏萌达新材料科技有限公司 | A kind of iron cobalt-copper alloy powder and preparation method thereof |
| CN110773750A (en) * | 2019-12-16 | 2020-02-11 | 重庆优钛新材料科技有限公司 | Method and device for preparing high-purity superfine metal powder |
| CN111872414A (en) * | 2020-06-12 | 2020-11-03 | 辽宁科技大学 | Preparation method of micro-nano pre-alloyed powder |
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| JPS5651506A (en) * | 1980-07-18 | 1981-05-09 | Mitsubishi Metal Corp | Production of high-speed steel powder |
| CN101011746A (en) * | 2007-02-07 | 2007-08-08 | 钢铁研究总院 | Method of manufacturing micro and sub-micron iron powder |
| CN101134243A (en) * | 2007-09-26 | 2008-03-05 | 中南大学 | Ultra-fine or nanometer molybdenum cuprum composite powder and method of producing the alloy thereof |
| CN101214553A (en) * | 2008-01-02 | 2008-07-09 | 中南大学 | Method for preparing ultra-fine/nano tungsten molybdenum copper composite powder |
| CN101823152A (en) * | 2010-04-14 | 2010-09-08 | 北京科技大学 | Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling |
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2014
- 2014-03-13 CN CN201310723092.1A patent/CN103817340A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5651506A (en) * | 1980-07-18 | 1981-05-09 | Mitsubishi Metal Corp | Production of high-speed steel powder |
| CN101011746A (en) * | 2007-02-07 | 2007-08-08 | 钢铁研究总院 | Method of manufacturing micro and sub-micron iron powder |
| CN101134243A (en) * | 2007-09-26 | 2008-03-05 | 中南大学 | Ultra-fine or nanometer molybdenum cuprum composite powder and method of producing the alloy thereof |
| CN101214553A (en) * | 2008-01-02 | 2008-07-09 | 中南大学 | Method for preparing ultra-fine/nano tungsten molybdenum copper composite powder |
| CN101823152A (en) * | 2010-04-14 | 2010-09-08 | 北京科技大学 | Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104128613A (en) * | 2014-08-20 | 2014-11-05 | 丹阳市德源精密工具有限公司 | Preparation method for pre-alloyed powder |
| CN105345020A (en) * | 2015-11-15 | 2016-02-24 | 丹阳市德源精密工具有限公司 | Preparation method for pre-alloyed powder |
| CN109702217A (en) * | 2019-03-04 | 2019-05-03 | 江苏萌达新材料科技有限公司 | A kind of iron cobalt-copper alloy powder and preparation method thereof |
| CN110773750A (en) * | 2019-12-16 | 2020-02-11 | 重庆优钛新材料科技有限公司 | Method and device for preparing high-purity superfine metal powder |
| CN111872414A (en) * | 2020-06-12 | 2020-11-03 | 辽宁科技大学 | Preparation method of micro-nano pre-alloyed powder |
| CN111872414B (en) * | 2020-06-12 | 2023-03-21 | 辽宁科技大学 | Preparation method of micro-nano pre-alloyed powder |
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Application publication date: 20140528 |