CN100389916C - Method of preparing ultrafine alloy powder by coprecipitation coreduction - Google Patents
Method of preparing ultrafine alloy powder by coprecipitation coreduction Download PDFInfo
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- CN100389916C CN100389916C CNB2006100116925A CN200610011692A CN100389916C CN 100389916 C CN100389916 C CN 100389916C CN B2006100116925 A CNB2006100116925 A CN B2006100116925A CN 200610011692 A CN200610011692 A CN 200610011692A CN 100389916 C CN100389916 C CN 100389916C
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Abstract
The present invention provides a method for preparing ultrafine alloy powder by coprecipitation and coreduction, which belongs to the technical field for the preparation of metal alloy powder. First, precursor powder with various alloy compositions is prepared through liquid phase coprecipitation and is calcined to obtain nanometer metal oxide composite powder which is then reduced by using hydrogen or cracked ammonia in a reducing furnace of an industrial tube type, and the alloying process is completed during the reduction process simultaneously to obtain the ultrafine alloy powder. The present invention realizes the controllable granularity of the alloy powder, homogeneous distribution and excellent sintering characteristic, and is suitable for industrial production. The present invention has the advantages of realizing the controllable granularity of the alloy powder, homogeneous distribution, excellent sintering character, simple technology and equipment and low cost, and is suitable for industrial production.
Description
Technical field
The invention belongs to the metal alloy powders preparing technical field, a kind of method of preparing ultrafine alloy powder by coprecipitation coreduction particularly is provided.
Background technology
Powder and alloy powders thereof such as Fe, Co, Ni, Cu, Mo, as: Fe-Ni, Ni-Cu, Fe-Ni-Cu, Ni-Co, Fe-Ni-Mo etc. are widely used in the powder metallurgy all trades and professions.Atomization is the common method of preparation alloy powder, and its advantage is to synthesize the alloy powder of various compositions by melting, but the general granularity of alloy powder of atomization preparation is thicker, and sintering character is not fine.Some sintered metal products need be finished sintering under lower sintering temperature, thermal pressing sintering diamond tool for example, too high sintering temperature can cause adamantine graphitization, thus need to use granularity less than the alloy powder of 2～5 μ m to reduce sintering temperature.In power injection molding, meal and fine powder collocation are used, can increase substantially useful load.What is more important uses superfine alloy powder to have through the fine grain sintered metal product of low-temperature sintering gained that conventional goods are incomparable decide high strength and high tenacity, is the key technology that obtains the fine grain sintered metal product and prepare superfine alloy powder.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing ultrafine alloy powder by coprecipitation coreduction, realized the alloy powder controllable granularity, be evenly distributed, the sintering character excellence, and be applicable to suitability for industrialized production.
The present invention at first prepares the precursor powder of various alloying components by liquid phase coprecipitation, precursor powder obtains the nanosize metal oxide composite powder through calcining, again the nanosize metal oxide composite powder is reduced with hydrogen or cracked ammonium in industrial tubular type reduction furnace, finish alloying process simultaneously in reduction process, obtain superfine alloy powder.Concrete preparation technology is:
1. prepared by co-precipitation precursor powder
Nitrate, sulfate or chloride and the deionized water of soluble metal (Fe, Co, Ni, Cu, Mo) are configured to the aqueous solution.According to the needs of alloy powder composition, various metal quality ratios can be arbitrary proportion, and the concentration of each metal ion species is 0～10mol/L in the aqueous solution.With measuring pump above-mentioned aqueous metal salt is injected reactor, by stoichiometric proportion alkaline solution (as NaOH, ammoniacal liquor, ammonium carbonate etc.) being injected reactor then mixes with aqueous metal salt, adjust solution pH value＞8, reaction generates hydroxide or the carbonate coprecipitation of Fe, Co, Ni, Cu, Mo, sediment obtains the co-precipitation precursor powder through 3～5 washings, suction filtration.
If the impurity composition in the co-precipitation can directly decompose at calcination stage, for example: it is nickelous carbonate, cobalt carbonate and ammonium nitrate that Ni, Co nitrate add ammonium carbonate coprecipitation reaction product, ammonium nitrate can pass through calcining and decomposing, can omit washing step, and directly the co-precipitation that suction filtration is obtained is calcined.
2. the calcining presoma prepares the nano-metal-oxide composite powder
With precursor powder in Muffle furnace 150～400 ℃ temperature lower calcination 1～4 hour, purpose is to make moisture evaporation, impurity, hydroxide or carbonate decomposition obtain the nano-metal-oxide composite powder.
3. coreduction prepares alloy powder
The nano-metal-oxide composite powder is reduced with hydrogen or cracked ammonium in industrial tubular type reduction furnace, and reduction temperature is 400～1000 ℃, and the cross section flow of hydrogen or cracked ammonium is 10～40ml/cm
2Min, the high-temperature region time of staying is 30～90 minutes, the metal that is reduced out is finished alloying process by diffusion under reduction temperature, obtain alloy powder.Can be by regulating the granularity of reduction temperature and hydrogen flowing quantity control reduzate alloy powder, obtaining particle mean size is the alloy powder of 0.8～5.0 μ m.
4. product treatment
Come out of the stove the back product because granularity is thinner, and the surface can be big, and activity is very high, and oxidation and increase oxygen content easily, even spontaneous combustion should spray into 5～15ml acetone-oleic acid mixed liquor with every kg powder immediately, and Vacuum Package.
The invention has the advantages that:
(1) but provide a kind of large-scale industrialization to produce the new technology of alloy powder from production technology;
(2) technology, equipment are simple, and cost is low;
(3) but in the hydrogen reduction range of metal, be applicable to the production of any composition proportion alloy powder;
(4) the alloy powder fine size of Sheng Chaning, even particle size distribution, sintering character excellence.
(5) the alloy powder controllable granularity of Sheng Chaning.
The specific embodiment
Embodiment 1: with nine water ferric nitrate (Fe (NO
3)
39H
2O), six water nickel nitrate (Ni (NO
3)
26H
2O) and ammoniacal liquor be raw material, prepare ultra-fine Fe75-Ni25 alloy powder, should finish as follows:
1. press mass ratio (Fe (NO
3)
39H
2O): (Ni (NO
3)
26H
2O)=541: 114 ratio takes by weighing raw material, adds deionized water, is configured to Fe
3+Concentration is 1.34 mol/L, Ni
2+Concentration is the aqueous solution of 0.43mol/L.With measuring pump this solution is injected reactor.Adding 2.44L concentration in 1L ferric nitrate nickel solution is the ratio of the ammoniacal liquor of 2mol/L, injects ammoniacal liquor in reactor by measuring pump, is stirred, and adjusts solution pH value＞8, and reacting generates the hydroxide co-precipitation of iron, nickel.
2. precipitation at 300 ℃ temperature lower calcination 2h, decomposes the hydroxide of iron, nickel and ammonium nitrate in suction filtration moves into Muffle furnace, obtains nano-level iron, ni compound oxide powder.
3. nano-level iron, ni compound oxide powder are reduced with hydrogen (or cracked ammonium) in the tubular type reduction furnace.Can obtain the superfine alloy powder of 0.8～5.0 μ m by adjustment reduction temperature, hydrogen flowing quantity, temperature retention time.For example: at reduction temperature is 1000 ℃, hydrogen cross section flow 20ml/cm
2Min, under the condition of high-temperature region holdup time 30min, can obtain particle mean size is the ultra-fine Fe75-Ni25 alloy powder of 5 μ m; At reduction temperature is 800 ℃, hydrogen cross section flow 20ml/cm
2Min, under the condition of high-temperature region holdup time 40min, can obtain particle mean size is the ultra-fine Fe75-Ni25 alloy powder of 2.5 μ m; At reduction temperature is 600 ℃, hydrogen cross section flow 30ml/cm
2Min, under the condition of high-temperature region holdup time 60min, can obtain particle mean size is the ultra-fine Fe75-Ni25 alloy powder of 1.5 μ m; At reduction temperature is 400 ℃, hydrogen cross section flow 40ml/cm
2Min, under the condition of high-temperature region holdup time 90min, can obtain particle mean size is the ultra-fine Fe75-Ni25 alloy powder of 0.8 μ m.
4. the back product of coming out of the stove sprays into 10ml acetone-oleic acid mixed liquor and Vacuum Package with every kg powder immediately, prevents oxidation and spontaneous combustion.
Embodiment 2: with anhydrous slufuric acid iron (Fe
2(SO
4)
3), anhydrous nickel sulfate NiSO
4Reaching NaOH (NaOH) is raw material, prepares ultra-fine Fe70-Ni30 alloy powder, should finish as follows:
1. press mass ratio Fe
2(SO
4)
3: NiSO
4=250: 79 ratio takes by weighing raw material, adds deionized water, is configured to Fe
3+Concentration is 1.25mol/L, Ni
2+Concentration is the aqueous solution of 0.51mol/L.With measuring pump this solution is injected reactor.Adding 2.39L concentration in 1L ferric sulfate nickel solution is the ratio of the sodium hydroxide solution of 2mol/L, injects sodium hydroxide solution in reactor by measuring pump, is stirred, and adjusts solution pH value＞8, and reacting generates the hydroxide co-precipitation of iron, nickel.
2. will precipitate suction filtration, and add the deionized water washing, BaCl is used in suction filtration, washing circulation several times again
2Solution detects the 8O in the filtrate
4 2-Ion is to filtrate SO
4 2-Till concentration is reduced to and can not detects.
3. the suction filtration postprecipitation moves in the Muffle furnace, and the temperature lower calcination 2h at 150 ℃ makes moisture evaporation, and the hydroxide of iron, nickel decomposes, and obtains nano-level iron, ni compound oxide powder.
4. with embodiment 1 step 3.Can obtain particle mean size is the ultra-fine Fe70-Ni30 alloy powder of 0.8～5.0 μ m.
5. with embodiment 1 step 4.
Embodiment 3: with six water nickel nitrate (Ni (NO
3)
26H
2O), cobalt nitrate hexahydrate (Co (NO
3)
26H
2O) and ammonium carbonate ((NH
4)
2CO
3H
2O) be raw material, prepare ultra-fine Ni80-Co20 alloy powder, should finish as follows:
1. press mass ratio (Ni (NO
3)
26H
2O): (Co (NO
3)
26H
2O)=4: 1 ratio takes by weighing raw material, adds deionized water, is configured to Ni
2+Concentration is 1.36mol/L, Co
2+Concentration is the aqueous solution of 0.34mol/L.By measuring pump this solution is injected reactor.Adding 1.75L concentration in the 1L nickel and cobalt solution is the ratio of the sal volatile of 1mol/L, injects sal volatile in reactor by measuring pump, is stirred, and adjusts solution pH value＞8, and reacting generates the carbonate coprecipitation of nickel, cobalt.
2. with embodiment 1 step 2, obtain nanoscale nickel, cobalt composite oxide powder.
3. with embodiment 1 step 3, can obtain particle mean size is the ultra-fine Ni80-Co20 alloy powder of 0.8～5.0 μ m.
4. with embodiment 1 step 4.
Embodiment 4: with ferric trichloride (FeCl
3), six water nickel chloride (NiCl
26H
2O), copper chloride dihydrate (CuCl
22H
2O) and NaOH (NaOH) be raw material, prepare ultra-fine Fe40-Ni20-Cu40 alloy powder, should finish as follows:
1. press mass ratio FeCl
3: (NiCl
26H
2O): (CuCl
22H
2O)=115: 81: 107 ratio takes by weighing raw material, adds deionized water, is configured to Fe
3+Concentration is 0.71mol/L, Ni
2+Concentration is 0.34mol/L, Cu
2+Concentration is 0.63mol/L, the aqueous solution.With measuring pump this solution is injected reactor.Adding 2.04L concentration in 1L iron chloride, nickel, copper solution is the ratio of the sodium hydroxide solution of 2mol/L, inject sodium hydroxide solution in reactor by measuring pump, stirred, adjust solution pH value＞8, reacting generates the hydroxide co-precipitation of iron, nickel.
2. will precipitate suction filtration, and add the deionized water washing, AgNO is used in suction filtration, washing circulation several times again
3Solution detects the Cl in the filtrate
-Ion is to liquor C l
-Till concentration is reduced to and can not detects.
3. the suction filtration postprecipitation moves in the Muffle furnace, and the temperature lower calcination 2h at 150 ℃ makes moisture evaporation, and the hydroxide of iron, nickel, copper decomposes, and obtains nano-level iron-nickel-copper composite oxide power.
4. with embodiment 1 step 3.Can obtain particle mean size is the ultra-fine Fe40-Ni20-Cu40 alloy powder of 0.8～5.0 μ m.
5. with embodiment 1 step 4.
Claims (1)
1. the method for a preparing ultrafine alloy powder by coprecipitation coreduction, it is characterized in that: preparation technology is:
A, prepared by co-precipitation precursor powder
The nitrate of 2 kinds among soluble metal Fe, Co, Ni, Cu, the Mo or multiple metal or sulfate or chloride and deionized water are configured to the aqueous solution, the concentration of each metal ion species is 0～10mol/L in the aqueous solution, in reactor, above-mentioned aqueous metal salt is mixed with alkaline solution, adjust solution pH value＞8, reaction generates hydroxide or the carbonate coprecipitation of corresponding Fe, Co, Ni, Cu, Mo, sediment obtains the co-precipitation precursor powder through 3～5 washings, suction filtration; Described alkaline solution is NaOH or ammoniacal liquor or ammonium carbonate;
B, calcining presoma prepare the nano-metal-oxide composite powder
With precursor powder in Muffle furnace 150～400 ℃ temperature lower calcination 1～4 hour, obtain the nano-metal-oxide composite powder;
C, coreduction prepare alloy powder
The nano-metal-oxide composite powder is reduced with hydrogen or cracked ammonium in industrial tubular type reduction furnace, and reduction temperature is 400～1000 ℃, and the cross section flow of hydrogen or cracked ammonium is 10～40ml/cm
2Min, temperature retention time is 30～90 minutes, and the metal that is reduced out is finished alloying process by diffusion under reduction temperature, obtain alloy powder, and particle mean size is the alloy powder of 0.8～5.0 μ m;
D, product treatment
After coming out of the stove, spray into 5～15ml acetone-oleic acid mixed liquor, Vacuum Package with every kilogram of powder.
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| CN100389916C true CN100389916C (en) | 2008-05-28 |
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Assignee: Beijing Ding Shi Century High Tech Co., Ltd. Assignor: University of Science and Technology Beijing Contract fulfillment period: 2008.9.20 to 2018.9.20 contract change Contract record no.: 2009990000306 Denomination of invention: Method of preparing ultrafine alloy powder by coprecipitation coreduction Granted publication date: 20080528 License type: Exclusive license Record date: 2009.4.13 |
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