CN105921762B - The Co-based alloy powder preparation method of shaping can be densified - Google Patents
The Co-based alloy powder preparation method of shaping can be densified Download PDFInfo
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- CN105921762B CN105921762B CN201610438436.8A CN201610438436A CN105921762B CN 105921762 B CN105921762 B CN 105921762B CN 201610438436 A CN201610438436 A CN 201610438436A CN 105921762 B CN105921762 B CN 105921762B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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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Abstract
The invention discloses a kind of Co-based alloy powder preparation method for being densified shaping, it is characterised in that comprises the steps：By mass percentage, component is weighed：Six water nickel nitrates 34.3~39.4%；Nine water chromic nitrates 23.9~26.9%, nine water ferric nitrates 1.7~2.2%, a water ammonium tungstate 2.5~3.1%, oxalic acid 30.7~35.4%；The water nickel nitrate of component six, nine water chromic nitrates and a water ammonium tungstate are first made into 300ml solution, 60~85 DEG C is heated to and stirs；2ml ammoniacal liquor is added, a few minutes are stirred；The water ferric nitrate of component nine and oxalic acid are added into solution, is incubated and stirs in water-bath；Solution is taken out, room temperature is naturally cooled to, filtering precipitation, by drying precipitate, is filtered and ground；Abrasive flour is loaded into corundum boat, 750 DEG C of reduction in hydrogen furnace is placed in, obtains Ni-base Superalloy Powder.
Description
Technical field
The present invention relates to the technology of preparing of alloy material, more particularly to a kind of preparation method of Co-based alloy powder.
Background technology
Nickel base superalloy be using nickel element as base, can more than 1200 DEG C at a high temperature of bear larger stress and with compared with
The alloy of high surface stability.It has the integration capability of preferable anti-oxidant, anticorrosive, creep resistant and fatigue at high temperature,
Available for the high temperature hot-end component for making aero-engine, rocket engine, naval vessels and industry gas turbine.Nickel is prepared at this stage
It is melting technique that the main method of based high-temperature alloy, which is thrown away, using elemental metals block, plate or band as raw material, by melting, casting etc.
Process obtains alloy, high energy consumption needed for preparing, and casting flaw easily occurs in alloy structure, increases subsequent treatment difficulty.To eliminate
The tissue defects of melting high temperature alloy, have scholar to prepare Ni-base Superalloy Powder using water atomization, use compacting sintering technology
By Alloy Forming.But the particle mean size of water atomized powder is larger, it is difficult to meet shaping densification and require.
The content of the invention
It is an object of the invention to provide a kind of preparation method for the nickel-bass alloy material for shaping alloy powder densification.
To achieve the above objectives, the present invention, which is adopted the following technical scheme that, is achieved,
A kind of Co-based alloy powder preparation method for being densified shaping, it is characterised in that comprise the steps：
(1) by mass percentage, component is weighed：Six water nickel nitrates 34.3~39.4%；Nine water chromic nitrates 23.9~
26.9%th, nine water ferric nitrates 1.7~2.2%, a water ammonium tungstate 2.5~3.1%, oxalic acid 30.7~35.4%；
(2) the water nickel nitrate of component six, nine water chromic nitrates and a water ammonium tungstate are first made into 300ml solution, it is heated to 60~
85 DEG C stir；
(3) 2ml ammoniacal liquor is added, a few minutes are stirred；
(4) the water ferric nitrate of component nine and oxalic acid are added into solution, is incubated and stirs in 65~75 DEG C of water-baths；
(5) solution is taken out, room temperature, filtering precipitation, by drying precipitate is naturally cooled to；
(6) by dried powder ethanol wash, filter and grind；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace and reduces, temperature is 750 DEG C, obtains nickel base superalloy
Powder.
In the above method, step (3) stirring is 5min.Step (4) stirring is 15~20min.
Step (5) described drying be put the precipitate in air dry oven in 180 DEG C dry 4 hours.
Step (6) grinding is that dried powder is milled to 0.8 μm of granularity.
Abrasive flour is reduced in step (7) described hydrogen furnace, 15 DEG C/minute of heating rate, soaking time cools after 5 hours,
10 DEG C/minute of rate of temperature fall.
Compared with prior art, the invention has the characteristics that and advantage：
1st, during Ni-base Superalloy Powder is prepared, the present invention is changed completely uses bulk metal in existing method
Melting, the thinking of atomization, but presoma is made with metal salt combination reaction, then prepare nickel base superalloy powder by reduction
End, and study solution acid alkalinity, bath temperature, reducing process and powder size and the relation of tissue.This method has equipment letter
Single, process controllability is strong and high efficiency, overcome because atomization gradation degree greatly caused by shaping densification ability problem.
2nd, the essential characteristic for preparing Ni-base Superalloy Powder presoma process aspect in chemical combination is：Pass through ionizable metal salt
Between complex reaction, shorten dissimilar metal atomic distance, be follow-up powder reduction, metal element alloyed offer basis.
3rd, the present invention prepares Ni-base Superalloy Powder with chemical combination-reducing process, and powder size≤0.2 μm of preparation has
Good crystallized ability.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
In each embodiment for preparing Ni-base Superalloy Powder below, powder size test condition meets《GB/T21524-
2008》Standard.
Embodiment 1
(1) 36.6 grams of six water nickel nitrate, 24.9 grams of nine water chromic nitrate, 1.86 grams of nine water ferric nitrate, a water ammonium tungstate are weighed
2.8 grams and 33.8 grams of oxalic acid；
(2) six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are first made into the 300ml aqueous solution, stirred with collection pyromagnetic force
Device heating, agitating solution are mixed, 15min, 900 revs/min of rotor speed are incubated in 60 DEG C of water-baths；
(3) 2ml ammoniacal liquor is added into solution, 5min, 900 revs/min of rotor speed is stirred；
(4) nine water ferric nitrates and oxalic acid are added into solution, is incubated 20min in 75 DEG C of water-baths, 1200 turns of rotor speed/
Point；
(5) solution is taken out, room temperature is naturally cooled to, precipitation is loaded ceramic crucible, in air dry oven by filtering precipitation
Dry 4 hours, 180 DEG C of temperature；
(6) by dried powder ethanol wash, filter and be ground to 0.8 μm of granularity；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace and reduces, obtain Ni-base Superalloy Powder, reduction temperature
750 DEG C of degree, 15 DEG C/minute of heating rate, 10 DEG C/minute of rate of temperature fall, soaking time 5 hours.
Embodiment 2
(1) 37.5 grams of six water nickel nitrate, 25.3 grams of nine water chromic nitrate, 1.62 grams of nine water ferric nitrate, a water ammonium tungstate are weighed
2.38 grams and 33.2 grams of oxalic acid；
(2) six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are first made into the 300ml aqueous solution, stirred with collection pyromagnetic force
Device heating, agitating solution are mixed, 15min, 1100 revs/min of rotor speed are incubated in 70 DEG C of water-baths；
(3) 2ml ammoniacal liquor is added into solution, 5min, 1100 revs/min of rotor speed is stirred；
(4) nine water ferric nitrates and oxalic acid are added into solution, is incubated 20min in 65 DEG C of water-baths, 1300 turns of rotor speed/
Point；
(5) solution is taken out, room temperature is naturally cooled to, precipitation is loaded ceramic crucible, in air dry oven by filtering precipitation
Dry 4 hours, 180 DEG C of temperature；
(6) by dried powder ethanol wash, filter and be ground to 0.8 μm of granularity；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace and reduces, obtain Ni-base Superalloy Powder, reduction temperature
750 DEG C of degree, 15 DEG C/minute of heating rate, 10 DEG C/minute of rate of temperature fall, soaking time 5 hours.
Embodiment 3
(1) 37.8 grams of six water nickel nitrate, 25.9 grams of nine water chromic nitrate, 2.1 grams of nine water ferric nitrate, a water ammonium tungstate are weighed
3.0 grams and 31.2 grams of oxalic acid；
(2) six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are first made into the 300ml aqueous solution, stirred with collection pyromagnetic force
Device heating, agitating solution are mixed, 15min, 1400 revs/min of rotor speed are incubated in 50 DEG C of water-baths；
(3) 2ml ammoniacal liquor is added into solution, 5min, 1400 revs/min of rotor speed is stirred；
(4) nine water ferric nitrates and oxalic acid are added into solution, is incubated 20min in 65 DEG C of water-baths, 1000 turns of rotor speed/
Point；
(5) solution is taken out, room temperature is naturally cooled to, precipitation is loaded ceramic crucible, in air dry oven by filtering precipitation
Dry 4 hours, 180 DEG C of temperature；
(6) by dried powder ethanol wash, filter and be ground to 0.8 μm of granularity；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace and reduces, obtain Ni-base Superalloy Powder, reduction temperature
750 DEG C of degree, 15 DEG C/minute of heating rate, 10 DEG C/minute of rate of temperature fall, soaking time 5 hours.
Embodiment 4
(1) 39.7 grams of six water nickel nitrate, 24.1 grams of nine water chromic nitrate, 1.8 grams of nine water ferric nitrate, a water ammonium tungstate are weighed
2.5 grams and 31.9 grams of oxalic acid；
(2) six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are first made into the 300ml aqueous solution, stirred with collection pyromagnetic force
Device heating, agitating solution are mixed, 15min, 1300 revs/min of rotor speed are incubated in 60 DEG C of water-baths；
(3) 2ml ammoniacal liquor is added into solution, 5min, 1300 revs/min of rotor speed is stirred；
(4) nine water ferric nitrates and oxalic acid are added into solution, is incubated 20min in 75 DEG C of water-baths, 1200 turns of rotor speed/
Point；
(5) solution is taken out, room temperature is naturally cooled to, precipitation is loaded ceramic crucible, in air dry oven by filtering precipitation
Dry 4 hours, 180 DEG C of temperature；
(6) by dried powder ethanol wash, filter and be ground to 0.8 μm of granularity；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace and reduces, obtain Ni-base Superalloy Powder, reduction temperature
750 DEG C of degree, 15 DEG C/minute of heating rate, 10 DEG C/minute of rate of temperature fall, soaking time 5 hours.
Performance to nickel base superalloy obtained by above example is tested, and is as a result listed in table 1.
Table 1 not be the same as Example prepare Ni-base Superalloy Powder performance parameter
| Sample number into spectrum | Granularity/μm |
| Embodiment 1 | 0.14 |
| Embodiment 2 | 0.19 |
| Embodiment 3 | 0.2 |
| Embodiment 4 | 0.13 |
As can be seen from Table 1, the Ni-base Superalloy Powder prepared with embodiment 1-4 methods has the characteristics of granularity is small.
The present invention is according to the thinking for changing metal element alloyed mode, by accurately controlling metal salt concentration, chemical combination, going back
Former technique reduces Ni-base Superalloy Powder granularity, and obtained Ni-base Superalloy Powder has preferable cold-press moulding performance,
As listed in table 2.
The cold-press moulding performance of the different Ni-base Superalloy Powders for implementing to prepare of table 2
| Sample number into spectrum | It is cold-pressed blank porosity/% |
| Embodiment 1 | 1.1 |
| Embodiment 2 | 0.4 |
| Embodiment 3 | 0.6 |
| Embodiment 4 | 0.9 |
As can be seen from Table 2, with the blank of embodiment 1-4 powder cold-press mouldings, porosity is low, base substrate is fine and close, formability
Can be good.
Claims (3)
1. a kind of Co-based alloy powder preparation method for being densified shaping, it is characterised in that comprise the steps：
(1) by mass percentage, component is weighed：Six water nickel nitrates 34.3~39.4%；Nine water chromic nitrates 23.9~26.9%, nine
Water ferric nitrate 1.7~2.2%, a water ammonium tungstate 2.5~3.1%, oxalic acid 30.7~35.4%；
(2) the water nickel nitrate of component six, nine water chromic nitrates and a water ammonium tungstate are first made into 300ml solution, are heated to 60~85 DEG C
Stir；
(3) 2ml ammoniacal liquor is added, a few minutes are stirred；
(4) the water ferric nitrate of component nine and oxalic acid are added into solution, is incubated and stirs in 65~75 DEG C of water-baths；
(5) solution is taken out, room temperature, filtering precipitation, by drying precipitate is naturally cooled to；
(6) by dried powder ethanol wash, filter and grind, grinding is that dried powder is milled to 0.8 μm of granularity；
(7) abrasive flour is loaded into corundum boat, is placed in hydrogen furnace in 750 DEG C of reduction, obtains Ni-base Superalloy Powder, it is described
Abrasive flour is reduced in hydrogen furnace, 15 DEG C/minute of heating rate, soaking time cools after 5 hours, 10 DEG C/minute of rate of temperature fall.
2. the Co-based alloy powder preparation method of shaping can be densified as claimed in claim 1, it is characterised in that step (3)
The stirring is 5min；Step (4) stirring is 15~20min.
3. the Co-based alloy powder preparation method of shaping can be densified as claimed in claim 1, it is characterised in that step (5)
The drying be put the precipitate in air dry oven in 180 DEG C dry 4 hours.
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| CN110961651A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of chromium-doped superfine nickel powder |
| CN110961649A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of cobalt-doped superfine nickel powder |
| CN110961654A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of tin-doped superfine nickel powder |
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| CN110961653A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of copper-doped superfine nickel powder |
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| CN110961650A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of zirconium-doped superfine nickel powder |
| CN110961655A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of tungsten-doped superfine nickel powder |
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| DE19622097A1 (en) * | 1996-06-01 | 1997-12-04 | Treibacher Ind Ag | Iron@-molybdenum@ alloy |
| JPH11124606A (en) * | 1997-10-22 | 1999-05-11 | Sumitomo Metal Mining Co Ltd | Nickel-copper alloy powder and its manufacture |
| CN101837464B (en) * | 2009-08-28 | 2012-12-26 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
| CN102649161B (en) * | 2011-02-23 | 2014-11-05 | 荆门市格林美新材料有限公司 | Nickel powder with large furnace safety supervision system (FSSS) particle size and preparation method thereof |
| CN102909383B (en) * | 2011-08-03 | 2015-08-05 | 深圳市格林美高新技术股份有限公司 | The preparation method of extra-fine nickel powder or cobalt powder |
| CN102601379A (en) * | 2012-03-29 | 2012-07-25 | 金川集团有限公司 | Method for preparing porous spherical nickel powder |
| CN104651653B (en) * | 2015-01-31 | 2016-11-23 | 陕西理工学院 | A kind of preparation method of the high-strength tungsten-nickel-copper alloy of microalloying of rare earth high density |
| CN105268983B (en) * | 2015-10-21 | 2017-09-22 | 陕西理工学院 | The preparation method of W Ni Cu pre-alloyed powders |
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