CN105921762A - Densification formation type preparation method of nickel-based alloy powder - Google Patents
Densification formation type preparation method of nickel-based alloy powder Download PDFInfo
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- CN105921762A CN105921762A CN201610438436.8A CN201610438436A CN105921762A CN 105921762 A CN105921762 A CN 105921762A CN 201610438436 A CN201610438436 A CN 201610438436A CN 105921762 A CN105921762 A CN 105921762A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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 densification formation type preparation method of nickel-based alloy powder. The method is characterized by comprising the following steps: weighting the following components in percentage by mass: 34.3 to 39.4% of nickelous nitrate hexahydrate, 23.9 to 26.9% of chromic nitrate nonahydrate, 1.7 to 2.2% of iron nitrate nonahydrate, 2.5 to 3.1% of ammonium tungstate monohydrate, and 30.7 to 35.4% of oxalic acid; preparing a 300mol solution through nickelous nitrate hexahydrate, chromic nitrate nonahydrate, and ammonium tungstate monohydrate, then heating to reach the temperature of 60 to 85 DEG C, and uniformly stirring; adding 2ml ammonium hydroxide, and stirring for a few minutes; adding iron nitrate nonahydrate and oxalic acid to the solution; maintaining the temperature in a water bath, and uniformly stirring; moving out the solution; naturally cooling to reach the room temperature; filtering and precipitating; drying, filtering and grinding the precipitate; placing the grinded powder into a corundum boat-shaped container; transferring the corundum boat-shaped container into a hydrogenation furnace to reduce at the temperature of 750 DEG C, so as to obtain high-temperature nickel-based alloy powder.
Description
Technical field
The present invention relates to the technology of preparing of alloy material, particularly to the preparation method of a kind of Co-based alloy powder.
Background technology
Nickel base superalloy is with nickel element as base, can bear under the high temperature more than 1200 DEG C and more greatly should
Power also has the alloy of high surfaces stability.Its at high temperature have preferable antioxidation, anticorrosive,
Creep resistant and tired integration capability, can be used for making aero-engine, rocket engine, naval vessels and
The high-temperature hot end pieces of industry gas turbine.Present stage prepares the main method of nickel base superalloy and throws away
Melting technique, with elemental metals block, plate or band as raw material, obtains through operations such as melted, castings
Alloy, the required energy consumption of preparation is high, and casting flaw easily occurs in alloy structure, increases subsequent treatment difficulty.
For eliminating the tissue defects of melting high temperature alloy, scholar is had to use water atomization to prepare nickel base superalloy
Powder, by compacting sintering technology by Alloy Forming.But the particle mean size of water atomized powder is bigger, it is difficult to
Meet and shape densification requirement.
Summary of the invention
It is an object of the invention to provide the system of a kind of nickel-bass alloy material making alloy powder densification shape
Preparation Method.
For reaching object above, the present invention adopts the following technical scheme that and is achieved,
A kind of can densification shape Co-based alloy powder preparation method, it is characterised in that include following step
Rapid:
(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%, one water ammonium tungstate 2.5～3.1%, oxalic acid 30.7～35.4%；
(2) first component six water nickel nitrate, nine water chromic nitrates and a water ammonium tungstate are made into 300ml solution, add
Heat stirs to 60～85 DEG C；
(3) add 2ml ammonia, stir a few minutes；
(4) component nine water ferric nitrate and oxalic acid are added solution, be incubated in 65～75 DEG C of water-baths and stir
Uniformly；
(5) take out solution, naturally cool to room temperature, filter precipitation, by drying precipitate；
(6) by dried powder ethanol wash, filtration and grind；
(7) abrasive flour loading corundum boat, be placed in hydrogen furnace reduction, temperature is 750 DEG C, obtains Ni-based
Superalloy powder.
In said method, step (3) described stirring is 5min.Step (4) described stirring is 15～20min.
Described being dried of step (5) is to put the precipitate in air dry oven to dry 4 hours in 180 DEG C.
Step (6) described grinding is the granularity that dried powder is milled to 0.8 μm.
Reduction abrasive flour in step (7) described hydrogen furnace, heating rate 15 DEG C/minute, temperature retention time 5 is little
Lower the temperature time after, rate of temperature fall 10 DEG C/minute.
Compared with prior art, the invention have the characteristics that and advantage:
1, during preparing Ni-base Superalloy Powder, the present invention changes employing block in existing method completely
Body metal melting, the thinking of atomization, but prepare presoma by slaine combination reaction, then through reduction system
Standby Ni-base Superalloy Powder, and study solution acid alkalinity, bath temperature, reducing process and powder size and
The relation of tissue.It is simple that the method has equipment, and process controllability is strong and high efficiency, overcomes because of atomization point
The difficult problem shaping densification ability that granularity causes greatly.
2, preparing the essential characteristic of Ni-base Superalloy Powder presoma process aspect at chemical combination is: pass through metal
Complex reaction between salt ion, shortens dissimilar metal atomic distance, for follow-up powder reduction, metallic element alloy
Change and basis is provided.
3, present invention chemical combination reducing process prepares Ni-base Superalloy Powder, and the powder size of preparation≤
0.2 μm, has good crystallized ability.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Hereinafter preparing in each embodiment of Ni-base Superalloy Powder, powder size test condition meets " GB/T
21524-2008 " standard.
Embodiment 1
(1) weigh six water nickel nitrate 36.6 grams, nine water chromic nitrate 24.9 grams, nine water ferric nitrate 1.86 grams, one
Water ammonium tungstate 2.8 grams and oxalic acid 33.8 grams；
(2) first six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are made into 300ml aqueous solution, with collection
The heating of pyromagnetic force agitator, agitating solution, be incubated 15min, rotor speed 900 revs/min in 60 DEG C of water-baths；
(3) in solution, add 2ml ammonia, stir 5min, rotor speed 900 revs/min；
(4) nine water ferric nitrates and oxalic acid are added solution, 75 DEG C of water-baths are incubated 20min, rotor speed
1200 revs/min；
(5) take out solution, naturally cool to room temperature, filter precipitation, precipitation is loaded ceramic crucible, is rousing
Wind drying baker is dried 4 hours, temperature 180 DEG C；
(6) by dried powder ethanol wash, filtration and be ground to 0.8 μm granularity；
(7) abrasive flour is loaded corundum boat, is placed in hydrogen furnace reduction, obtains Ni-base Superalloy Powder,
Reduction temperature 750 DEG C, heating rate 15 DEG C/minute, rate of temperature fall 10 DEG C/minute, temperature retention time 5 hours.
Embodiment 2
(1) weigh six water nickel nitrate 37.5 grams, nine water chromic nitrate 25.3 grams, nine water ferric nitrate 1.62 grams, one
Water ammonium tungstate 2.38 grams and oxalic acid 33.2 grams；
(2) first six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are made into 300ml aqueous solution, with collection
The heating of pyromagnetic force agitator, agitating solution, insulation 15min in 70 DEG C of water-baths, rotor speed 1100 turns/
Point；
(3) in solution, add 2ml ammonia, stir 5min, rotor speed 1100 revs/min；
(4) nine water ferric nitrates and oxalic acid are added solution, 65 DEG C of water-baths are incubated 20min, rotor speed
1300 revs/min；
(5) take out solution, naturally cool to room temperature, filter precipitation, precipitation is loaded ceramic crucible, is rousing
Wind drying baker is dried 4 hours, temperature 180 DEG C；
(6) by dried powder ethanol wash, filtration and be ground to 0.8 μm granularity；
(7) abrasive flour is loaded corundum boat, is placed in hydrogen furnace reduction, obtains Ni-base Superalloy Powder,
Reduction temperature 750 DEG C, heating rate 15 DEG C/minute, rate of temperature fall 10 DEG C/minute, temperature retention time 5 hours.
Embodiment 3
(1) weigh six water nickel nitrate 37.8 grams, nine water chromic nitrate 25.9 grams, nine water ferric nitrate 2.1 grams, one
Water ammonium tungstate 3.0 grams and oxalic acid 31.2 grams；
(2) first six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are made into 300ml aqueous solution, with collection
The heating of pyromagnetic force agitator, agitating solution, insulation 15min in 50 DEG C of water-baths, rotor speed 1400 turns/
Point；
(3) in solution, add 2ml ammonia, stir 5min, rotor speed 1400 revs/min；
(4) nine water ferric nitrates and oxalic acid are added solution, 65 DEG C of water-baths are incubated 20min, rotor speed
1000 revs/min；
(5) take out solution, naturally cool to room temperature, filter precipitation, precipitation is loaded ceramic crucible, is rousing
Wind drying baker is dried 4 hours, temperature 180 DEG C；
(6) by dried powder ethanol wash, filtration and be ground to 0.8 μm granularity；
(7) abrasive flour is loaded corundum boat, is placed in hydrogen furnace reduction, obtains Ni-base Superalloy Powder,
Reduction temperature 750 DEG C, heating rate 15 DEG C/minute, rate of temperature fall 10 DEG C/minute, temperature retention time 5 hours.
Embodiment 4
(1) weigh six water nickel nitrate 39.7 grams, nine water chromic nitrate 24.1 grams, nine water ferric nitrate 1.8 grams, one
Water ammonium tungstate 2.5 grams and oxalic acid 31.9 grams；
(2) first six water nickel nitrates, nine water chromic nitrates and a water ammonium tungstate are made into 300ml aqueous solution, with collection
The heating of pyromagnetic force agitator, agitating solution, insulation 15min in 60 DEG C of water-baths, rotor speed 1300 turns/
Point；
(3) in solution, add 2ml ammonia, stir 5min, rotor speed 1300 revs/min；
(4) nine water ferric nitrates and oxalic acid are added solution, 75 DEG C of water-baths are incubated 20min, rotor speed
1200 revs/min；
(5) take out solution, naturally cool to room temperature, filter precipitation, precipitation is loaded ceramic crucible, is rousing
Wind drying baker is dried 4 hours, temperature 180 DEG C；
(6) by dried powder ethanol wash, filtration and be ground to 0.8 μm granularity；
(7) abrasive flour is loaded corundum boat, is placed in hydrogen furnace reduction, obtains Ni-base Superalloy Powder,
Reduction temperature 750 DEG C, heating rate 15 DEG C/minute, rate of temperature fall 10 DEG C/minute, temperature retention time 5 hours.
Being tested the performance of above example gained nickel base superalloy, result is listed in table 1.
The performance parameter of Ni-base Superalloy Powder prepared by the different embodiment of table 1
| 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, it is little that the Ni-base Superalloy Powder prepared by embodiment 1-4 method has granularity
Feature.
The present invention is according to the thinking of the metal element alloyed mode of change, by accurately controlling metal salt concentration, change
Close, reducing process reduces Ni-base Superalloy Powder granularity, and the Ni-base Superalloy Powder obtained has preferably
Cold-press moulding performance, as listed in table 2.
The cold-press moulding performance of the different Ni-base Superalloy Powder implementing preparation of table 2
| Sample number into spectrum | Cold pressing 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 moulding, porosity is low, base substrate is fine and close,
Forming property is good.
Claims (5)
1. one kind can densification shape Co-based alloy powder preparation method, it is characterised in that include following
Step:
(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%, one water ammonium tungstate 2.5～3.1%, oxalic acid 30.7～35.4%；
(2) first component six water nickel nitrate, nine water chromic nitrates and a water ammonium tungstate are made into 300ml solution, add
Heat stirs to 60～85 DEG C；
(3) add 2ml ammonia, stir a few minutes；
(4) component nine water ferric nitrate and oxalic acid are added solution, be incubated in 65～75 DEG C of water-baths and stir
Uniformly；
(5) take out solution, naturally cool to room temperature, filter precipitation, by drying precipitate；
(6) by dried powder ethanol wash, filtration and grind；
(7) abrasive flour is loaded corundum boat, be placed in hydrogen furnace in 750 DEG C of reduction, obtain nickel-base high-temperature and close
Bronze end.
The most as claimed in claim 1 can the Co-based alloy powder preparation method that shapes of densification, it is special
Levying and be, step (3) described stirring is 5min；Step (4) described stirring is 15～20min.
The most as claimed in claim 1 can the Co-based alloy powder preparation method that shapes of densification, it is special
Levying and be, described being dried of step (5) is to put the precipitate in air dry oven to dry 4 hours in 180 DEG C.
The most as claimed in claim 1 can the Co-based alloy powder preparation method that shapes of densification, it is special
Levying and be, step (6) described grinding is the granularity that dried powder is milled to 0.8 μm.
The most as claimed in claim 1 can the Co-based alloy powder preparation method that shapes of densification, it is special
Levy and be, reduction abrasive flour, heating rate 15 DEG C/minute, temperature retention time in step (7) described hydrogen furnace
Lower the temperature after 5 hours, rate of temperature fall 10 DEG C/minute.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN110961647A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of molybdenum-doped superfine nickel powder |
| 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 |
| 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 |
| 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 |
| 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 |
| CN110961652A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of lanthanum-doped superfine nickel powder |
| CN110961648A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of titanium-doped superfine nickel powder |
| CN110961658A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of iron-doped superfine nickel powder |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN110961647A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of molybdenum-doped superfine nickel powder |
| 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 |
| 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 |
| 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 |
| 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 |
| CN110961652A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of lanthanum-doped superfine nickel powder |
| CN110961648A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of titanium-doped superfine nickel powder |
| CN110961658A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of iron-doped superfine nickel powder |
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