CN109877312A - A kind of preparation method of spherical shape ferrite base ODS alloy powder - Google Patents
A kind of preparation method of spherical shape ferrite base ODS alloy powder Download PDFInfo
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Abstract
The invention belongs to spherical metal based powders preparation research fields, provide a kind of preparation method of spherical ferrite base ODS alloy powder, the specific steps are, nano oxidized material resource is dissolved in solvent and stirs to get clear solution, aerosolization powder is added in clear solution, and it is mixed 0.5-4 hours under 20-60 revs/min of revolving speed using batch mixer, obtain precursor pulp, precursor pulp is subjected to radio frequency plasma nodularization, precursor pulp conveys atomizer by carrier gas, the high-temperature region nitrate that radio frequency plasma heating is reached after being atomized decomposes to obtain corresponding oxide nano-particles first, then atomized powder and oxide nano-particles, which are heated by radio frequency plasma, melts, then become spherical under the action of surface tension, and spherical ODS ferrite base powder is obtained through supercooling.The present invention provides new thinking for preparation spherical shape ODS ferrite base powder, has many advantages, such as with short production cycle, at low cost, easy to operate.
Description
Technical field
The invention belongs to spherical metal based powders preparation research fields, specifically provide a kind of spherical shape ferrite base ODS conjunction
The preparation method of the method at bronze end.
Background technique
Oxide dispersion intensifying (Oxides Dispersion strengthening, ODS) Alfer has good
Mechanical property, mechanical behavior under high temperature, creep-resistant property and shoulder irradiation behaviour, in auto industry, aerospace and nuclear industry etc.
There is important application prospect in field.
ODS ferrite mainly carries out dispersion-strengtherning by very tiny nanometer oxide particle (cluster).Due to nano oxygen
Compound particle generally has high thermal stability, and will not be dissolved in matrix in high temperature, therefore it has further promotion alloy military service
The potentiality of temperature.Meanwhile the nanometer oxide particle of high-volume fractional can effectively promote its anti-radiation damage and swell with anti-radiation
Swollen ability.Therefore the size of nanometer oxide particle, number density and stability are to determine the key factor of its service performance
(Journal of Nuclear Materials, 2017,486:11-20).ODS Alfer is mainly closed by Cr, W, Mo etc.
The nanometer oxide particles formation element such as gold element and Y, Ti, O composition.Wherein Cr, W, Mo, etc. alloying elements mainly to play solid solution strong
Change the effect of matrix, Cr can also promote alloy corrosion ability.Y, the addition of Ti, O element will form Y2Ti2O7Equal combined oxidations
Object, and nano-oxide size can be further refined, promote alloy property.
The exploitation of ODS Alfer and its always international research hot spot of advanced forming technique.Powder injection forming
The representative technology of technology and 3D printing technique as powder near-net-shape, is suitable for the forming of moderate dimensions, complex shape part.
Due to at low cost, precision is high, few cutting is even without series of advantages, Powder Injection Molding Technology and 3D printing skills such as cuttings
Art preparation ODS Alfer has received widespread attention.In order to guarantee the complete of complicated fine structure during near-net-shape
Property, the powder of usual powder injection forming and 3D printing needs spherical powder to guarantee its mobility and filling capacity.
However the preparation of ODS Alfer powder mainly uses mechanical alloying method at present.Mechanical alloying technique system
When the oxide dispersion strengthening ferrite based alloy that standby intermetallic compound and oxide are strengthened jointly, the metallic elements such as Fe, Cr
It is easy to aoxidize in ma process, promotes alloy oxygen content, performance decline.Meanwhile prolonged ball milling is easy to draw
Enter being mingled with for ball-milling medium material, reduces the mechanical behavior under high temperature of material.Finally, most of the powder that mechanical alloying obtains is
Powder in irregular shape, powder flowbility are poor.This causes it that can not carry out by the methods of 3D printing or powder injection forming
Near-net-shape.This strictly limits the application for the Alfer that intermetallic compound and nano-oxide are strengthened jointly.Therefore,
A kind of technology of preparing of method for preparing spherical ferrite base ODS alloy powder must be developed.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing spherical ferrite base ODS alloy powder, it is intended to develop one
Kind high efficiency method prepares spherical, with superfine oxide disperse phase ferrite base powder.Spherical ODS ferrite base powder
Designability is strong, dispersed oxide is mutually especially tiny.
The present invention uses the atomized powder of subject alloy and corresponding oxide nitrate solution to prepare powder precursor first, connects
Powder precursor is prepared into the slurry with certain fluidity, then by precursor pulp with radio frequency plasma nodularization obtain
Spherical ODS ferrite base powder.
Therefore, the present invention provides a kind of method for preparing spherical ferrite base ODS alloy powder, and the method includes as follows
Step,
The configuration of S1 precursor pulp: with Y (NO3)2·6H2O or La (NO3)2·6H2One of O is nano oxidized material resource, molten
Clear solution is stirred to get in appropriate solvent, by Fe- (6-20wt.%) Cr- (0.1-5wt.%) W- (0-2wt.%) Mo- (0.1-
1wt.%) Ti aerosolization powder is added in clear solution, exists until alloy powder is just soaked by alcohol, and using batch mixer
Mixed 0.5-4 hours under 20-60 revs/min of revolving speed, the precursor pulp being uniformly mixed, the nano oxidized material resource and
The dosage of aerosolization powder is so that the nano-oxide in the powder being finally prepared accounts for the quality hundred of ODS ferrite base powder
Dividing content is 0.01-5wt.%；
S2. the preparation of spherical shape ODS ferrite base powder-product: carrying out radio frequency plasma nodularization for obtained precursor pulp, preceding
It drives somaplasm material and atomizer is conveyed by carrier gas, the high-temperature region nitrate that radio frequency plasma heating is reached after being atomized occurs to divide first
Solution obtains corresponding oxide nano-particles, and then atomized powder and oxide nano-particles are heated by radio frequency plasma molten
Change, then becomes spherical under the action of surface tension, and obtain spherical ODS ferrite base powder through supercooling.
In a kind of specific embodiment, in step a, the ingredient of aerosolization powder is Fe- (6-20wt.%) Cr- (0.1-
5wt.%) W- (0-2wt.%) Mo- (0.1-2wt.%) Ti, the wherein preferred 8-16 wt.% of Cr content, the preferred 0.3-3 of W content
The preferred 0-1.5 wt.% of wt.%, Mo content, the preferred 0.1-1 wt.% of Ti content, Fe is surplus.
In a kind of specific embodiment, solvent is alcohol in S1.
In a kind of specific embodiment, S1, nano oxidized material resource is Y (NO3)3·6H2O and La (NO3)3·6H2In O
One kind, final nano-oxide account for ODS ferrite base powder mass percentage be 0.01-5wt.%, preferably 0.1-
1wt.%。
In a kind of specific embodiment, the carrier gas in S2 is argon gas, carrier gas flux 1-10L/min, preferably carrier gas
Flow is 4-8L/min.
In a kind of specific embodiment, the middle gas in S2 is argon gas, and middle throughput is 15-40L/min, preferably middle gas
Flow is 20-30L/min.
In a kind of specific embodiment, the shell gas in S2 is argon gas, and shell throughput is 65-100L/min, preferably shell
Throughput is 70-80L/min.
In a kind of specific embodiment, the precursor pulp rate of feed in S2 is 20-200g/min, preferably 50-
150g/min。
In a kind of specific embodiment, the intracavitary negative pressure in S2 is 6000-16000Pa, preferably 6500-13500Pa.
The advantages of the present invention:
1, spherical shape ODS ferrite base powder sphericity obtained in the present invention is high, has more tiny nanoscale oxygen in spherical powder
Compound disperse phase is distributed wherein.
2, the designability of the invention for preparing product is strong, and not only product composition is controllable, and the partial size and sphericity of product can also
By technology controlling and process appropriate, and nano oxide dispersion is mutually especially tiny.
3, simple process in the present invention can directly directly obtain spherical target powder from precursor pulp, compared to
Mechanical alloy+radio frequency plasma nodularization method is a kind of preparation method of efficient spherical shape ODS ferrite base powder.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the preparation method of spherical ferrite base ODS alloy powder of the invention.
Fig. 2 is the structural schematic diagram of spherical shape ODS ferrite base powder preparing unit.
Specific embodiment
Technical scheme is described further combined with specific embodiments below.
As shown in Figure 1, a kind of preparation method of spherical ferrite base ODS alloy powder of the present invention, the method includes such as
Lower step,
The configuration of S1 precursor pulp: nano-oxide is added after appropriate solvent and stirs to get clear solution, by aerosolization
Until being completely soaked in powder addition clear solution, mixed 0.5-4 hours under 20-60 revs/min of revolving speed using batch mixer,
The precursor pulp being uniformly mixed；
The preparation of S2 spherical shape ODS ferrite base powder-product: the precursor pulp that S1 is obtained uses radio frequency plasma nodularization skill
Art nodularization obtains spherical ferrite base ODS alloy powder.
According to the embodiment of the present disclosure, the additional amount of the nano oxidized material resource is that spherical ferrite base is finally prepared
Nano-oxide in ODS alloy powder accounts for the 0.01-5wt.% of the mass percent of ODS ferrite base powder.
According to the embodiment of the present disclosure, it can also be that spherical ferrite base is finally prepared that the nano oxidized material resource, which is added,
Nano-oxide in ODS alloy powder accounts for 0. 1-1wt.% of the mass percent of ODS ferrite base powder.
According to the embodiment of the present disclosure, solvent is alcohol in the S1.
According to the embodiment of the present disclosure, the component of aerosolization powder in the S1 are as follows: Cr:6-20wt.%, W:0.1-5wt.%,
Mo0-2wt.%, Ti:0.1-2wt.%, surplus Fe.
According to the embodiment of the present disclosure, the component of aerosolization powder in the S1 are as follows: Cr:8-16 wt.%, W:0.3-3 wt.%,
Mo:0-1.5 wt.%, Ti:0.1-1 wt.%, surplus Fe.
According to the embodiment of the present disclosure, nano oxidized material resource is Y (NO in the S13)3·6H2O or La (NO3)3·6H2In O
One kind.
Radio frequency plasma spheronization techniques specific process parameter according to the embodiment of the present disclosure, in the S2 are as follows: carrier gas is argon
Gas, carrier gas flux 1-10L/min；Middle gas is argon gas, and middle throughput is 15-40L/min；Shell throughput is 65-100L/min；
Precursor pulp rate of feed is 20-200g/min.
According to the embodiment of the present disclosure, the radio frequency plasma spheronization techniques specific process parameter in the S2 may be used also are as follows: carrier gas
Flow is 4-8L/min；Middle gas is argon gas, and middle throughput is 20-30L/min；Shell throughput is 70-80L/min；Forerunner's somaplasm
Material rate of feed is 50-150g/min.
A kind of spherical ferrite base ODS alloy powder that the method is prepared is applied to powder injection forming or 3D
Printing technique field.
Embodiment 1:
Fe-12.3wt.%Cr-0.39wt.%Ti-0.25wt.%Y2O3The preparation of spherical ODS ferrite base powder
The atomized powder and yttrium nitrate (Y (NO for being Fe-12.3wt.%Cr-0.39wt.%Ti by ingredient3)3·6H2O) with mass ratio
117.616:1 weighing good spare.Load weighted yttrium nitrate is dissolved in suitable alcohols, stir evenly in a reservoir to be formed it is transparent molten
Liquid.Atomized powder and suitable alcohol are uniformly added into solution again, until alloy powder is just soaked by alcohol.Then make
It is mixed 2 hours under 45 revs/min of revolving speed with batch mixer, obtains precursor pulp.During radio frequency plasma nodularization, negative pressure
For 7800Pa；Middle gas is argon gas, and middle throughput is 15L/min；Shell gas is argon gas, and shell throughput is 65L/min；It is flowed with 4L/min
Precursor solution is sprayed into plasma arc through feed system, feeding gun for carrier gas with the charging rate of 135g/min by the argon gas of amount
In, precursor pulp finally enters cooling chamber and condenses rapidly in the moment endothermic decomposition melting then nodularization in plasma arc.?
It is 10.6nm, the Fe-12.3wt.%Cr-0.39wt.%Ti- that powder average particle size is 180 μm to nano-oxide average grain diameter
0.25wt.%Y2O3Spherical ODS ferrite base powder.
Embodiment 2:
Fe-14wt.%Cr-1wt.%Ti-0.3Mo-0.5wt.%La2O3The preparation of spherical ODS ferrite base powder
The atomized powder and lanthanum nitrate (La (NO for being Fe-14wt.%Cr-1wt.%Ti-0.3Mo by ingredient3)3·6H2O) with mass ratio
74.866:1 weighing good spare.Load weighted lanthanum nitrate is first dissolved in suitable alcohols, stir evenly in a reservoir to be formed it is transparent molten
Liquid.Atomized powder and suitable alcohol are uniformly added into solution again, until alloy powder is just soaked by alcohol.Then make
It is mixed 3 hours under 30 revs/min of revolving speed with batch mixer, obtains precursor pulp.During radio frequency plasma nodularization, negative pressure
For 8500Pa；Middle gas is argon gas, and middle throughput is 22L/min；Shell gas is argon gas, and shell throughput is 70L/min；It is flowed with 6L/min
The argon gas of amount is that carrier gas sprays into precursor solution in plasma arc through feed system, feeding gun with the charging rate of 90g/min,
Precursor pulp finally enters cooling chamber and condenses rapidly in the moment endothermic decomposition melting then nodularization in plasma arc.It obtains
Nano-oxide average grain diameter is 9.5nm, the Fe-14wt.%Cr-1wt.%Ti-0.3Mo- that powder average particle size is 120 μm
0.5wt.%La2O3Spherical ODS ferrite base powder.
Embodiment 3:
Fe-14wt.%Cr-0.2wt.%Ti-0.3wt.%Y2O3The preparation of spherical ODS ferrite base powder
By ingredient be Fe-14wt.%Cr-0.2wt.%Ti atomized powder and with yttrium nitrate (Y (NO3)3·6H2O) with mass ratio
97.965:1 weighing good spare.Load weighted yttrium nitrate is first dissolved in suitable alcohols, stir evenly in a reservoir to be formed it is transparent molten
Liquid.Atomized powder and suitable alcohol are uniformly added into solution again, until alloy powder is just soaked by alcohol.Then make
It is mixed 1 hour under 60 revs/min of revolving speed with batch mixer, obtains precursor pulp.During radio frequency plasma nodularization, negative pressure
For 9000Pa；Middle gas is argon gas, and middle throughput is 25L/min；Shell gas is argon gas, and shell throughput is 75L/min；It is flowed with 7L/min
The argon gas of amount is that carrier gas sprays into precursor solution in plasma arc through feed system, feeding gun with the charging rate of 80g/min,
Precursor pulp finally enters cooling chamber and condenses rapidly in the moment endothermic decomposition melting then nodularization in plasma arc.It obtains
Nano-oxide average grain diameter is 8.4nm, the Fe-14wt.%Cr-0.2wt.%Ti-0.3wt.% that powder average particle size is 90 μm
Y2O3Spherical ODS ferrite base powder.
Embodiment 4:
Fe-14wt.%Cr-3wt.%W-0.4wt.%Ti-0.25wt.%Y2O3The preparation of spherical ODS ferrite base powder
The atomized powder and yttrium nitrate (Y (NO for being Fe-14wt.%Cr-3wt.%W-0.4wt.%Ti by ingredient3)3·6H2O) with quality
It has been weighed than 117.616:1 spare.Load weighted yttrium nitrate is first dissolved in suitable alcohols, stir evenly in a reservoir to be formed it is transparent
Solution.Atomized powder and suitable alcohol are uniformly added into solution again, until alloy powder is just soaked by alcohol.Then
It is mixed 4 hours under 20 revs/min of revolving speed using batch mixer, obtains precursor pulp.During radio frequency plasma nodularization, bear
Pressure is 10000Pa；Middle gas is argon gas, and middle throughput is 30L/min；Shell gas is argon gas, and shell throughput is 80L/min；With 8L/
Precursor solution is sprayed into plasma through feed system, feeding gun for carrier gas with the charging rate of 50g/min by the argon gas of min flow
In arc, precursor pulp finally enters cooling chamber and condenses rapidly in the moment endothermic decomposition melting then nodularization in plasma arc.
Obtaining nano-oxide average grain diameter is 6.5nm, the Fe-14wt.%Cr-3wt.%W-0.4wt.% that powder average particle size is 50 μm
Ti-0.25wt.%Y2O3Spherical ODS ferrite base powder.
The above content is combine specific preferred embodiment to the further description of the invention made, and it cannot be said that originally
The specific implementation of invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, not
Under the premise of being detached from present inventive concept, several simple deductions and replacement can also be made, all shall be regarded as belonging to guarantor of the invention
Protect range.
Claims (10)
1. a kind of preparation method of spherical shape ferrite base ODS alloy powder, which is characterized in that described method includes following steps,
The configuration of S1 precursor pulp: nano oxidized material resource being added in appropriate solvent and stirs to get clear solution, then by aerosol
Change until being completely soaked in powder addition clear solution, is being stirred using batch mixer, the forerunner's somaplasm being uniformly mixed
Material；
The preparation of S2 spherical shape ODS ferrite base powder-product: the precursor pulp that S1 is obtained uses radio frequency plasma nodularization skill
Art nodularization obtains spherical ferrite base ODS alloy powder.
2. preparation method according to claim 1, which is characterized in that the additional amount of the nano oxidized material resource is final system
The standby nano-oxide obtained in spherical ferrite base ODS alloy powder accounts for the mass percent of ODS ferrite base powder
0.01-5wt.%.
3. preparation method according to claim 2, which is characterized in that the nano oxidized material resource, which is added also, to be final system
The standby nano-oxide obtained in spherical ferrite base ODS alloy powder accounts for the quality hundred of spherical ferrite base ODS alloy powder
Divide the 0.1-1wt.% of ratio.
4. the method according to claim 1, wherein in the S1 aerosolization powder component are as follows: Cr:6-
20wt.%, W:0.1-5wt.%, Mo:0-2wt.%, Ti:0.1-2wt.%, surplus Fe.
5. according to the method described in claim 4, it is characterized in that, in the S1 aerosolization powder component are as follows: Cr:8-
16wt.%, W:0.3-3wt.%, Mo:0-1.5wt.%, Ti:0.1-1wt.%, surplus Fe.
6. the method according to claim 1, wherein nano-oxide is Y (NO in a steady stream in the S13)3·6H2O
Or La (NO3)3·6H2O。
7. the method according to claim 1, wherein the radio frequency plasma spheronization techniques concrete technology in the S2
Parameter are as follows: carrier gas is argon gas, carrier gas flux 1-10L/min；Middle gas is argon gas, and middle throughput is 15-40L/min；Shell air-flow
Amount is 65-100L/min；Precursor pulp rate of feed is 20-200g/min.
8. the method according to the description of claim 7 is characterized in that the radio frequency plasma spheronization techniques concrete technology in the S2
Parameter may be used also are as follows: carrier gas flux 4-8L/min；Middle gas is argon gas, and middle throughput is 20-30L/min；Shell throughput is 70-
80L/min；Precursor pulp rate of feed is 50-150g/min.
9. the method according to claim 1, wherein the solvent in the S1 is alcohol；The batch mixer turns
Speed is 20-60 revs/min, and mixing time is 0.5-4 hours.
10. a kind of spherical ferrite base ODS alloy powder being prepared such as any one of claim 1~9 the method
Be applied to powder injection forming or 3D printing technique field.
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| CN112064011A (en) * | 2020-08-27 | 2020-12-11 | 北京科技大学 | Method for preparing multi-nano-phase reinforced ferrite alloy with complex shape |
| CN112063910A (en) * | 2020-08-27 | 2020-12-11 | 湘潭大学 | Method for preparing ODS ferrite-based alloy and application thereof |
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