CN109877312B - Preparation method of spherical ferrite-based ODS alloy powder - Google Patents
Preparation method of spherical ferrite-based ODS alloy powder Download PDFInfo
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Abstract
The invention belongs to the field of preparation research of spherical metal-based powder, and provides a preparation method of spherical ferrite-based ODS alloy powder, which comprises the following specific steps of dissolving a nano oxide source in a solvent, stirring to obtain a transparent solution, adding gas atomized powder into the transparent solution, mixing for 0.5-4 hours at a rotating speed of 20-60 r/min by using a mixer to obtain precursor slurry, carrying out radio frequency plasma spheroidization on the precursor slurry, conveying the precursor slurry to an atomizing nozzle by carrier gas, atomizing, allowing the atomized precursor slurry to reach a high-temperature region heated by radio frequency plasma, decomposing nitrate to obtain corresponding oxide nanoparticles, heating and melting the atomized powder and the oxide nanoparticles by the radio frequency plasma, changing the atomized powder and the oxide nanoparticles into spheres under the action of surface tension, and cooling to obtain the spherical ODS ferrite-based powder. The invention provides a new idea for preparing spherical ODS ferrite-based powder, and has the advantages of short production period, low cost, convenient operation and the like.
Description
Technical Field
The invention belongs to the field of preparation research of spherical metal-based powder, and particularly provides a preparation method of spherical ferrite-based ODS alloy powder.
Background
The Oxide Dispersion Strengthened (ODS) ferrite alloy has good mechanical property, high-temperature mechanical property, creep resistance and irradiation-carrying property, and has important application prospect in the fields of automobile industry, aerospace, nuclear industry and the like.
The ODS ferrite is mainly dispersion-strengthened by very fine nano-oxide particles (clusters). The nano oxide particles generally have high thermal stability and are not dissolved in a matrix at high temperature, so that the nano oxide particles have the potential of further increasing the service temperature of the alloy. Meanwhile, the nano-oxide particles with high volume fraction can effectively improve the radiation damage resistance and radiation swelling resistance. The size, number density and stability of the nano-oxide particles are critical factors in determining their performance (Journal of Nuclear Materials, 2017, 486: 11-20). The ODS ferrite alloy is mainly composed of alloy elements such as Cr, W and Mo, and elements formed by nano-oxide particles such as Y, Ti and O. Wherein, the alloy elements of Cr, W, Mo, etc. mainly play the role of solid solution strengthening matrix, and Cr can also improve the corrosion resistance of the alloy. Addition of Y, Ti, O elements will form Y2Ti2O7And the size of the nano oxide can be further refined, and the alloy performance is improved.
The development of ODS ferrite alloy and its advanced forming technology have been the hot points of international research. Powder injection molding technology and 3D printing technology are taken as representative technologies of powder near-net shaping, and are suitable for shaping parts with moderate size and complex shapes. Because of a series of advantages of low cost, high precision, less cutting and even no cutting, the preparation of ODS ferrite alloy by the powder injection molding technology and the 3D printing technology is receiving wide attention. In order to ensure the integrity of complex fine structures during near net shape forming, powders for powder injection molding and 3D printing generally require spherical powders to ensure their flowability and filling properties.
However, the current ODS ferritic alloy powder is mainly prepared by using a mechanical alloying method. When the oxide dispersion strengthened ferrite-based alloy jointly strengthened by the intermetallic compound and the oxide is prepared by the mechanical alloying process, the metal elements such as Fe, Cr and the like are easy to be oxidized in the mechanical alloying process, so that the oxygen content of the alloy is improved, and the performance is reduced. Meanwhile, the inclusion of the ball milling medium material is easily introduced by long-time ball milling, and the high-temperature mechanical property of the material is reduced. Finally, the powder obtained by mechanical alloying is mostly irregular in shape and poor in powder flowability. This makes it impossible to perform near-net shape forming by methods such as 3D printing or powder injection molding. This severely limited the use of ferritic alloys with co-strengthening of intermetallic compounds and nano-oxides. Therefore, it is necessary to develop a preparation technique for a method of preparing a spherical ferrite-based ODS alloy powder.
Disclosure of Invention
The invention aims to provide a method for preparing spherical ferrite-based ODS alloy powder, and aims to develop an efficient method for preparing spherical ferrite-based powder with an ultrafine oxide dispersed phase. The spherical ODS ferrite-based powder has strong designability and extremely fine oxide dispersed phase.
The method comprises the steps of firstly preparing a powder precursor by adopting atomized powder of a target alloy and a corresponding oxide nitrate solution, then preparing the powder precursor into slurry with certain fluidity, and then spheroidizing the precursor slurry by using radio frequency plasma to obtain spherical ODS ferrite-based powder.
Accordingly, the present invention provides a method for preparing a spherical ferrite-based ODS alloy powder, comprising the steps of,
preparation of S1 precursor slurry: with Y (NO)3)2·6H2O or La (NO)3)2·6H2One of O is a nano oxide source, the nano oxide source is dissolved in a proper amount of solvent and stirred to obtain a transparent solution, Fe- (6-20wt.%) Cr- (0.1-5wt.%) W- (0-2wt.%) Mo- (0.1-1wt.%) Ti atomized gas powder is added into the transparent solution until the alloy powder is just soaked by alcohol, and the mixture is mixed for 0.5-4 hours at the rotating speed of 20-60 r/min by using a mixer to obtain uniformly mixed precursor slurry, wherein the nano oxide source and the atomized gas powder are used in such amounts that the nano oxide in the finally prepared powder accounts for 0.01-5wt.% of the ODS ferrite-based powder;
s2, preparing a spherical ODS ferrite-based powder product: and (2) carrying out radio frequency plasma spheroidization on the obtained precursor slurry, conveying the precursor slurry to an atomizing nozzle by carrier gas, atomizing, then decomposing nitrate in a high-temperature region heated by radio frequency plasma to obtain corresponding oxide nano particles, heating and melting the atomized powder and the oxide nano particles by the radio frequency plasma, then changing the atomized powder and the oxide nano particles into spheres under the action of surface tension, and cooling to obtain spherical ODS ferrite-based powder.
In a specific embodiment, in step a, the composition of the aerosolized powder is Fe- (6-20wt.%) Cr- (0.1-5wt.%) W- (0-2wt.%) Mo- (0.1-2wt.%) Ti, wherein the Cr content is preferably 8-16 wt.%, the W content is preferably 0.3-3 wt.%, the Mo content is preferably 0-1.5 wt.%, the Ti content is preferably 0.1-1wt.%, and the balance is Fe.
In a specific embodiment, the solvent in S1 is an alcohol.
In one specific embodiment, S1, the source of nano-oxides is Y (NO)3)3·6H2O and La (NO)3)3·6H2And one of O, wherein the final nano oxide accounts for 0.01-5 wt%, preferably 0.1-1 wt% of the ODS ferrite-based powder.
In a specific embodiment, the carrier gas in S2 is argon, and the carrier gas flow is 1-10L/min, preferably 4-8L/min.
In a specific embodiment, the gas used in S2 is argon, and the flow rate of the gas is 15-40L/min, preferably 20-30L/min.
In a specific embodiment, the shell gas in S2 is argon, the shell gas flow is 65-100L/min, and the preferred shell gas flow is 70-80L/min.
In a specific embodiment, the precursor slurry feed rate in S2 is 20-200g/min, preferably 50-150 g/min.
In a specific embodiment, the negative pressure in the chamber in S2 is 6000-16000Pa, preferably 6500-13500 Pa.
The invention has the advantages and beneficial effects that:
1. the spherical ODS ferrite-based powder obtained by the method has high sphericity, and the spherical powder has finer nano-scale oxide dispersion phase distributed therein.
2. The product prepared by the invention has strong designability, the product components are controllable, the particle size and the sphericity of the product can be controlled by a proper process, and the dispersed phase of the nano oxide is extremely fine.
3. The method has simple process, can directly obtain the spherical target powder from the precursor slurry, and is an efficient preparation method of the spherical ODS ferrite-based powder compared with a mechanical alloy and radio frequency plasma spheroidization method.
Drawings
FIG. 1 is a process flow diagram of a method for preparing spherical ferrite-based ODS alloy powder according to the present invention.
FIG. 2 is a schematic view showing the structure of a spherical ODS ferrite-based powder preparation apparatus.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
As shown in FIG. 1, a method for preparing a spherical ferrite-based ODS alloy powder according to the present invention comprises the steps of,
preparation of S1 precursor slurry: adding a proper amount of solvent into the nano oxide, stirring to obtain a transparent solution, adding the gas atomized powder into the transparent solution until the gas atomized powder is completely soaked, and mixing for 0.5 to 4 hours at a rotating speed of 20 to 60 revolutions per minute by using a mixer to obtain uniformly mixed precursor slurry;
preparation of S2 spherical ODS ferrite-based powder product: and spheroidizing the precursor slurry obtained in the step S1 by adopting a radio frequency plasma spheroidization technology to obtain spherical ferrite-based ODS alloy powder.
According to the embodiment of the disclosure, the nano-oxide source is added in an amount of 0.01-5wt.% of the nano-oxides in the finally prepared spherical ferrite-based ODS alloy powder based on the mass percent of the ODS ferrite-based powder.
According to the embodiment of the disclosure, the addition of the nano-oxide source can also be 0.1-1wt.% of the mass percentage of the nano-oxides in the finally prepared spherical ferrite-based ODS alloy powder to the ODS ferrite-based powder.
According to an embodiment of the present disclosure, the solvent in S1 is alcohol.
According to the embodiment of the disclosure, the components of the atomized gas powder in S1 are: cr: 6-20wt.%, W: 0.1-5wt.%, Mo0-2wt.%, Ti: 0.1-2wt.%, the balance being Fe.
According to the embodiment of the disclosure, the components of the atomized gas powder in S1 are: cr: 8-16 wt.%, W: 0.3-3 wt.%, Mo: 0-1.5 wt.%, Ti: 0.1-1wt.%, the balance being Fe.
According to the embodiment of the disclosure, the nano-oxide source in S1 is Y (NO)3)3·6H2O or La (NO)3)3·6H2And O is one of the compounds.
According to the embodiment of the present disclosure, the specific process parameters of the radio frequency plasma spheroidization technique in S2 are as follows: the carrier gas is argon, and the flow rate of the carrier gas is 1-10L/min; the middle gas is argon, and the flow rate of the middle gas is 15-40L/min; the shell gas flow is 65-100L/min; the feeding speed of the precursor slurry is 20-200 g/min.
According to the embodiment of the present disclosure, the specific process parameters of the radio frequency plasma spheroidization technique in S2 may also be: the carrier gas flow is 4-8L/min; the middle gas is argon, and the flow rate of the middle gas is 20-30L/min; the shell gas flow is 70-80L/min; the feeding speed of the precursor slurry is 50-150 g/min.
The spherical ferrite-based ODS alloy powder prepared by the method is applied to the technical field of powder injection molding or 3D printing.
Example 1:
Fe-12.3wt.%Cr-0.39wt.%Ti-0.25wt.%Y2O3preparation of spherical ODS ferrite-based powder
Atomized powder with Fe-12.3wt.% Cr-0.39wt.% Ti and yttrium nitrate (Y (NO)3)3·6H2O) was weighed out in a mass ratio of 117.616:1 for use. Dissolving weighed yttrium nitrate into a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 2 hours at a rotation speed of 45 rpm using a mixer to obtain precursor slurry. In the process of spheroidization of the radio-frequency plasma,the negative pressure is 7800 Pa; the middle gas is argon, and the flow rate of the middle gas is 15L/min; the shell gas is argon, and the shell gas flow is 65L/min; argon gas with the flow rate of 4L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 135g/min, and precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidized and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 10.6nm, and the powder has an average particle size of 180 μm, and contains Fe-12.3wt.% Cr-0.39wt.% Ti-0.25wt.% Y2O3Spherical ODS ferrite-based powder.
Example 2:
Fe-14wt.%Cr-1wt.%Ti-0.3Mo-0.5wt.%La2O3preparation of spherical ODS ferrite-based powder
Atomized powder with Fe-14wt.% Cr-1wt.% Ti-0.3Mo and lanthanum nitrate (La (NO)3)3·6H2O) was weighed out in a mass ratio of 74.866:1 for use. Firstly, dissolving weighed lanthanum nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 3 hours at a rotation speed of 30 rpm by using a mixer to obtain precursor slurry. In the process of radio frequency plasma spheroidization, the negative pressure is 8500 Pa; the middle gas is argon, and the flow rate of the middle gas is 22L/min; the shell gas is argon, and the shell gas flow is 70L/min; argon gas with the flow rate of 6L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 90g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 9.5nm, and the powder has an average particle size of 120 μm, and contains Fe-14wt.% Cr-1wt.% Ti-0.3Mo-0.5wt.% La2O3Spherical ODS ferrite-based powder.
Example 3:
Fe-14wt.%Cr-0.2wt.%Ti-0.3wt.%Y2O3preparation of spherical ODS ferrite-based powder
Atomized powder containing Fe-14wt.% Cr-0.2wt.% Ti and yttrium nitrate (Y (NO)3)3·6H2O) is weighed according to the mass ratio of 97.965:1The dosage is good for standby. Firstly, dissolving weighed yttrium nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 1 hour at a rotation speed of 60 rpm using a mixer to obtain precursor slurry. In the process of radio frequency plasma spheroidization, the negative pressure is 9000 Pa; the middle gas is argon, and the flow rate of the middle gas is 25L/min; the shell gas is argon, and the shell gas flow is 75L/min; argon gas with the flow rate of 7L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 80g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 8.4nm, and the powder has an average particle size of 90 μm, and contains Fe-14wt.% Cr-0.2wt.% Ti-0.3wt.% Y2O3Spherical ODS ferrite-based powder.
Example 4:
Fe-14wt.%Cr-3wt.%W-0.4wt.%Ti-0.25wt.%Y2O3preparation of spherical ODS ferrite-based powder
Atomized powder with Fe-14wt.% Cr-3wt.% W-0.4wt.% Ti and yttrium nitrate (Y (NO)3)3·6H2O) was weighed out in a mass ratio of 117.616:1 for use. Firstly, dissolving weighed yttrium nitrate in a proper amount of alcohol, and uniformly stirring in a container to form a transparent solution. And uniformly adding the atomized powder and a proper amount of alcohol into the solution until the alloy powder is just soaked by the alcohol. And then mixed for 4 hours at a rotation speed of 20 rpm by using a mixer to obtain precursor slurry. In the process of radio frequency plasma spheroidization, the negative pressure is 10000 Pa; the middle gas is argon, and the flow rate of the middle gas is 30L/min; the shell gas is argon, and the shell gas flow is 80L/min; argon gas with the flow rate of 8L/min is used as carrier gas, precursor solution is sprayed into a plasma arc through a feeding system and a feeding gun at the feeding speed of 50g/min, precursor slurry is instantaneously subjected to heat absorption, decomposition and melting in the plasma arc, then spheroidizing, and finally enters a cooling chamber for rapid condensation. The obtained nano oxide has an average particle size of 6.5nm, powder has an average particle size of 50 μm, and Fe-14wt.% Cr-3wt.% W-0.4wt.% Ti-0.25wt.% Y2O3Spherical ODS ferrite-based powder.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions and substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. A method for producing a spherical ferrite-based ODS alloy powder, characterized by comprising the steps of,
preparation of S1 precursor slurry: adding a nano oxide source into a proper amount of solvent, stirring to obtain a transparent solution, adding gas atomized powder into the transparent solution until the gas atomized powder is completely soaked, and stirring again by using a mixer to obtain uniformly mixed precursor slurry; the addition amount of the nano oxide source ensures that the nano oxide in the spherical ferrite-based ODS alloy powder finally prepared accounts for 0.01-5wt.% of the mass percent of the ODS ferrite-based powder;
the nano oxide source is Y (NO)3)3·6H2O or La (NO)3)3·6H2O；
The gas atomization powder comprises the following components: cr: 6-20wt.%, W: 0.1-5wt.%, Mo: 0-2wt.%, Ti: 0.1-2wt.%, balance Fe;
preparation of S2 spherical ODS ferrite-based powder product: and spheroidizing the precursor slurry obtained in the step S1 by adopting a radio frequency plasma spheroidization technology to obtain spherical ferrite-based ODS alloy powder.
2. The method according to claim 1, wherein the source of nano-oxides is added in an amount that ensures that nano-oxides in the finally-prepared spherical ferrite-based ODS alloy powder account for 0.1-1wt.% of the mass percentage of the spherical ferrite-based ODS alloy powder.
3. The method of claim 1, wherein the composition of the aerosolized powder in S1 is: cr: 8-16 wt.%, W: 0.3-3 wt.%, Mo: 0-1.5 wt.%, Ti: 0.1-1wt.%, the balance being Fe.
4. The method of claim 1, wherein the specific process parameters of the rf plasma spheroidization technique in S2 are as follows: the carrier gas is argon, and the flow rate of the carrier gas is 1-10L/min; the middle gas is argon, and the flow rate of the middle gas is 15-40L/min; the shell gas flow is 65-100L/min; the feeding speed of the precursor slurry is 20-200 g/min.
5. The method of claim 4, wherein the specific process parameters of the RF plasma spheroidization technique in S2 are further: the carrier gas flow is 4-8L/min; the middle gas is argon, and the flow rate of the middle gas is 20-30L/min; the shell gas flow is 70-80L/min; the feeding speed of the precursor slurry is 50-150 g/min.
6. The method according to claim 1, wherein the solvent in S1 is alcohol; the rotating speed of the mixer is 20-60 r/min, and the stirring time is 0.5-4 hours.
7. Application of the spherical ferrite-based ODS alloy powder prepared by the method of any one of claims 1-6 in the technical field of powder injection molding or 3D printing.
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| CN101498034A (en) * | 2009-01-16 | 2009-08-05 | 中国科学院过程工程研究所 | Preparation of transient metal doped nano zinc oxide crystal whisker |
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