CN112063910B - Method for preparing ODS ferrite-based alloy and application thereof - Google Patents
Method for preparing ODS ferrite-based alloy and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
Abstract
The invention belongs to the field of preparation research of oxide dispersion strengthened alloy, and particularly provides a method for preparing ODS ferrite-based alloy by laser cladding forming and application thereof. The method comprises the following steps: preparation of precursor powder: the method comprises the steps of adding gas atomized ferrite-based alloy powder into a poly (diallyldimethylammonium chloride) solution or a cysteine solution for soaking for a period of time, then adding a nano oxide into the solution, stirring, and drying the solution. Preparing nano oxide coated ferrite alloy powder: and putting the obtained precursor powder into a high-speed stirring heating furnace, and stirring at a certain temperature under the condition of atmosphere protection to obtain the nano-oxide coated ferrite-based alloy powder. Performing laser cladding on the ferrite powder coated with the nano oxide to form the ODS ferrite-based alloy. The invention provides a new idea for preparing the ODS ferrite-based alloy, 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 oxide dispersion strengthened alloy, and particularly provides a method for preparing ODS ferrite-based alloy by laser cladding forming and application thereof.
Background
Due to the low density and thermal expansion coefficient, excellent mechanical property and radiation resistance, the ferrite-based alloy is widely applied to the fields of automobile industry, aerospace, nuclear industry and the like. However, as the use temperature increases, the mechanical properties of the ferritic base alloy, in particular the creep resistance, decrease drastically, which leads to a limitation in its use. In order to improve the high-temperature use performance of the ferrite-based alloy, an Oxide Dispersion Strengthened (ODS) ferrite alloy is formed by adding nano Oxides into a matrix, which is an effective method. Because oxides such as yttrium oxide, lanthanum oxide and the like have extremely high thermodynamic stability, when the oxide in a ferrite matrix is controlled in a nanometer scale through a proper process, the mechanical property and the radiation resistance of the ODS ferrite alloy are improved. And generally, the finer the grain size of the nano oxide is, the more the mechanical property and the radiation resistance of the ODS ferrite alloy are improved.
The advanced forming technology of complex-shaped ODS ferrite-based alloy products has been an international research focus. The laser cladding forming technology is taken as a representative technology of powder near-net forming and is suitable for forming parts with moderate size and complex shapes. Because of having a series of advantages such as low cost, high precision, little cutting even no cutting, the laser cladding forming technology for preparing ODS ferrite alloy has received extensive attention. In order to ensure the integrity of a complex fine structure in the near-net forming process, compared with the traditional process, the powder for laser cladding forming generally needs spherical fine-grained powder, and has higher requirements on the purity of the powder.
Conventional ODS ferrite-based alloys are generally prepared using a mechanical alloying method. When the oxide dispersion strengthening ferrite-based alloy is prepared by a mechanical alloying process, metal elements such as Fe, Cr and the like are easy to oxidize 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 seriously hardened, most of the powder is irregular in shape, the powder has poor flowability, and the powder can only be formed by some special methods such as sheath hot extrusion, sheath hot isostatic pressing or discharge plasma sintering, so that the requirement of a laser cladding forming technology on the powder cannot be met. Therefore, there is a need to develop a new technique for producing an ODS ferrite-based alloy product.
Disclosure of Invention
The invention aims to provide a method for preparing an ODS ferrite alloy, and aims to develop an efficient method for preparing the ODS ferrite alloy with ultra-fine oxide dispersion. The ODS ferrite alloy has strong designability and extremely fine and uniform oxide dispersed phases.
The invention firstly adopts atomized powder of target alloy and corresponding nano oxide to prepare powder precursor, and then the powder precursor is put into a special stirring heating furnace to obtain ferrite powder wrapped by dispersion phase of superfine oxide.
Therefore, the invention provides a method for preparing an ODS ferrite alloy, which comprises the following steps of, a, preparing precursor powder: firstly, the concentration is adjusted to be 4-10 g.L-1Adding the gas atomized powder of Fe- (8-18 wt.%) Cr- (0.1-5 wt.%) W- (0-2 wt.%) Nb- (0-1 wt.%) Ti into the solution, immersing for 10-30 min, and selecting nano Y2O3Or La2O3One of the powders is a nano oxide source, the nano oxide and the argon atomized FeCrWNbTi powder are added into the solution and stirred for 0.5 to 6 hours, and then the solution is dried, wherein the nano oxide and the argon atomized FeCrWNbTi powder are used in such an amount that the mass percentage of the nano oxide in the finally prepared powder in the ODS ferrite-based alloy is 0.01 to 5 wt.%. b. Preparing nano oxide coated ferrite alloy powder: and (b) putting the precursor powder obtained in the step (a) into a high-speed stirring heating furnace, carrying out high-speed stirring at a certain temperature under the condition of atmosphere protection, decomposing and removing organic matters remained in the precursor in the high-speed stirring process, breaking up the agglomeration of powder raw materials, and infiltrating the nano-oxide into the surface layer of the aerosol alloy powder particles to finally obtain the ferrite-based alloy powder coated by the nano-oxide. c. Carrying out laser cladding on ferrite powder coated with nano oxides to form an ODS ferrite alloy: c, performing laser cladding forming on the ferrite-based alloy powder coated with the nano oxides obtained in the step b, and controlling the laser cladding forming processThe process leads the metal powder to be melted by laser to form a molten pool, and leads the nanometer oxide to be brought into the molten pool and evenly dispersed and distributed by the flow of the liquefied metal in the molten pool, and finally the ODS ferrite alloy with the dispersion of the superfine oxide is obtained.
In a specific embodiment, in step a, the solution for preparing the precursor powder is poly (diallyldimethylammonium chloride) solution or cysteine solution with a concentration of 4-10 g.L-1Preferably 6 to 8 g.L-1。
In a specific embodiment, the composition of the argon atomized FeCrWNbTi powder in step a is Fe- (8-18 wt.%) Cr- (0.1-5 wt.%) W- (0-2 wt.%) Nb- (0-1 wt.%) Ti, wherein the Cr content is preferably 9-12 wt.%, the W content is preferably 0.3-3 wt.%, the Mo content is preferably 0-1.5 wt.%, the Ti content is preferably 0-0.5 wt.%, and the balance is Fe.
In a specific embodiment, in step a, the time for stirring after the powder raw material is added to the solution is 0.5 to 6 hours, preferably 0.5 to 2 hours.
In a specific embodiment, in step a, the source of nano-oxide is nano-Y2O3Or La2O3One of the powders, the final nano-oxide accounts for 0.01-5wt.%, preferably 0.1-1wt.% of the ODS ferrite-based powder.
In a specific embodiment, the protective atmosphere in step b is one of vacuum, argon and nitrogen, and preferably the protective atmosphere is vacuum and argon.
In a particular embodiment, the incubation temperature in step b is from 100 ℃ to 600 ℃, preferably from 200 ℃ to 400 ℃.
In a specific embodiment, the rotation speed of the stirring propeller in step b is 15000-.
In a particular embodiment, the stirring time in step b is from 0.5 to 4 hours, preferably from 0.5 to 2 hours.
In a specific embodiment, the laser scanning speed in step c is 500-.
In a specific embodiment, the laser scanning pitch in step c is 0.02 to 0.075mm, preferably 0.03 to 0.05 mm.
In a particular embodiment, the thickness of the dusting in step c is from 0.02 to 0.075mm, preferably from 0.03 to 0.05 mm.
The invention has the advantages that:
1. the invention provides a method for preparing ODS iron-based alloy by using SLM, which effectively solves the problems of poor flowability, low apparent density and difficulty in SLM forming of mechanically alloyed ODS iron-based powder, and provides a new idea for near-net forming of ODS iron-based alloy.
2. The ODS iron-based alloy obtained by the method has high density, and the dispersed phase particle size of the nano oxide is 5-20nm and is uniformly dispersed and distributed in a matrix.
3. The alloy prepared by the method has the advantages of high component designability and low cost, and can be used for preparing products with complex shapes under the condition of less processing or no processing.
Drawings
FIG. 1 is a process flow diagram of a method for preparing an ODS ferrite-based alloy according to the present invention.
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 an ODS ferrite-based alloy according to the present invention comprises the steps of:
s1) configuration of precursor powder: adding argon atomized FeCrWNbTi powder into the precursor solution, soaking, simultaneously adding a rare earth-containing nano oxide source, uniformly stirring, and drying to obtain precursor powder;
s2) heating the precursor powder obtained in the step S1) under the atmosphere protection condition to a set temperature, preserving heat, and stirring at a high speed to obtain ferrite-based alloy powder coated by nano oxides;
s3) performing laser cladding forming on the ferrite-based alloy powder coated with the nano-oxide obtained in S2), controlling the process to enable the metal powder to be melted by laser to form a molten pool, and bringing the nano-oxide into the molten pool by the flowing of liquefied metal in the molten pool and uniformly dispersing and distributing the nano-oxide to finally obtain the ODS ferrite-based alloy with ultra-fine oxide dispersion.
The S1) comprises the following specific steps:
s1.1) firstly preparing a precursor solution, and then adding argon atomized FeCrWNbTi powder into the precursor solution to dip for 10-30 minutes to obtain a suspension solution;
s1.2) selecting a rare earth-containing nano oxide source, adding the rare earth-containing nano oxide source into the suspension solution, stirring for 0.5-6 hours, drying the solution to obtain precursor powder,
wherein the rare earth nano oxide is used in an amount which ensures that the nano oxide in the finally prepared alloy accounts for 0.01-5 wt% of the ODS ferrite-based alloy.
The precursor solution is poly diallyl dimethyl ammonium chloride solution or cysteine with the concentration of 4-10 g.L-1；
The rare earth nano oxide source is Y2O3Or La2O3Powder;
the mass percentages of the components of the argon atomization FeCrWNbTi powder are as follows: cr: 8-18 wt.%; w: 0.1-5 wt.%; nb: 0-2 wt.%; ti: 0-1 wt.%; the balance being Fe.
The S2) comprises the following specific steps:
s2.1) placing the obtained precursor powder in a protective atmosphere for heating to 100-600 ℃;
s2.2) preserving the heat, and stirring for 0.5-4 hours by adopting a stirring propeller at the rotating speed of 15000-40000 r/min to obtain the nano-oxide coated ferrite-based alloy powder.
The protective atmosphere is argon, nitrogen or vacuum.
The S3) comprises the following specific steps:
s3.1) carrying out laser cladding forming on the obtained ferrite-based alloy powder coated with the nano oxides, wherein the powder laying thickness is 0.02-0.075 mm;
s3.2) laser scanning is adopted, the scanning speed is 500-4000mm/S, the scanning distance is 0.02-0.075mm, the flow of the liquefied metal in the molten pool brings the nano-oxide into the molten pool and the nano-oxide is uniformly dispersed and distributed, and finally the ODS ferrite-based alloy with the dispersion of the ultra-fine oxide is obtained.
The concentration of the precursor solution can also be 6-8 g.L-1；
The mass percentages of the components of the argon atomization FeCrWNbTi powder can also be as follows: 9-12 wt.% of Cr, 0.3-3 wt.% of W, 0-1.5 wt.% of Mo, 0-0.5 wt.% of Ti, and the balance of Fe; stirring for 0.5-2 hours;
the rare earth nano oxide is used in an amount which ensures that the nano oxide in the finally prepared alloy accounts for 0.1-1 wt% of the ODS ferrite-based alloy.
The heating temperature in the S2) can also be 200-400 ℃;
the rotation speed can also be 20000-30000 r/min, and the stirring time can be 0.5-2 hours.
In the S3), the powder spreading thickness can also be 0.03-0.05 mm; the scanning speed is 1000-2000 mm/s; the scanning interval can also be 0.03-0.05 mm.
The ODS ferrite-based alloy prepared by the method is applied to the fields of automobile industry, aerospace and nuclear industry.
Example 1: the composition Fe-9 wt.% Cr-2 wt.% W-0.4 wt.% Ti-0.35 wt.% Y2O3Preparation of ODS ferrite-based alloy
The components of the gas atomized powder are Fe-9 wt.% Cr-2 wt.% W-0.4 wt.% Ti and nano Y2O3The powder is weighed for standby according to the mass ratio of 99.65: 0.35. Dissolving the weighed gas atomized powder of Fe-9 wt.% Cr-2 wt.% W-0.4 wt.% Ti in 6 g.L-1The poly (diallyldimethylammonium chloride) solution is soaked for 30 minutes, and then the nano Y is added2O3Adding the powder into the solution, stirring for 0.5 hour, and drying the solution to obtain a powder precursor. And stirring the powder precursor for 1 hour in an argon atmosphere at the temperature of 300 ℃ and the rotating speed of a stirring propeller of 20000 revolutions per minute to obtain the nano-oxide coated ferrite-based alloy powder. Finally, carrying out laser cladding forming on the nano oxide coated ferrite-based alloy powder, wherein the forming parameters are that the powder laying thickness is 0.03mm, and the powder is sweptThe scanning speed is 1000mm/s, the scanning distance is 0.03mm, and the ODS ferrite-based alloy product with the target shape is obtained.
Example 2:
the composition Fe-12 wt.% Cr-2.1 wt.% W-0.5 wt.% Nb-0.3 wt.% Ti-0.25 wt.% Y2O3Preparation of ODS ferrite-based alloy
The components of the gas atomized powder are Fe-12 wt.% Cr-2.1 wt.% W-0.5 wt.% Nb-0.3 wt.% Ti and nano Y2O3The powder is weighed for standby according to the mass ratio of 99.75: 0.25. Dissolving the weighed gas atomized powder of Fe-12 wt.% Cr-2.1 wt.% W-0.5 wt.% Nb-0.3 wt.% Ti in 8 g.L-1The poly (diallyldimethylammonium chloride) solution is soaked for 20 minutes, and then the nano Y is added2O3Adding the powder into the solution, stirring for 1 hour, and drying the solution to obtain a powder precursor. And stirring the powder precursor for 2 hours in an argon atmosphere at the temperature of 300 ℃ and the rotating speed of a stirring propeller of 22000 r/min to obtain the nano-oxide coated ferrite-based alloy powder. And finally, carrying out laser cladding forming on the nano oxide coated ferrite-based alloy powder, wherein forming parameters comprise the powder laying thickness of 0.05mm, the scanning speed of 1200mm/s and the scanning distance of 0.05mm, and obtaining the ODS ferrite-based alloy product with the target shape.
Example 3: the composition Fe-9 wt.% Cr-1 wt.% W-0.3 wt.% Nb-1 wt.% La2O3Preparation of ODS ferrite-based alloy
The components of the gas atomized powder are Fe-9 wt.% Cr-1.5 wt.% W-1 wt.% Nb and nano La2O3The powder is weighed for standby according to the mass ratio of 99: 1. Dissolving the weighed gas atomized powder of Fe-9 wt.% Cr-1.5 wt.% W-1 wt.% Nb in 8 g.L-1The cysteine solution is soaked for 30 minutes, and then the nano La is added2O3And adding the powder into the solution, stirring for 2 hours, and drying the solution to obtain a powder precursor. And stirring the powder precursor for 1 hour in an argon atmosphere at the temperature of 500 ℃ and the rotating speed of a stirring propeller of 25000 r/min to obtain the nano-oxide coated ferrite-based alloy powder. Finally, carrying out laser cladding forming on the nano oxide coated ferrite-based alloy powder, wherein the forming parameters are that the powder laying thickness is 0.03mm, and the scanning speed is 1500mm/sAnd the scanning distance is 0.04mm, and the ODS ferrite-based alloy product with the target shape is obtained.
Example 3: the composition of Fe-12 wt.% Cr-2 wt.% W-0.8 wt.% Nb-0.5 wt.% La2O3Preparation of ODS ferrite-based alloy
The components of the gas atomized powder are Fe-12 wt.% Cr-2 wt.% W-0.8 wt.% Nb and nano La2O3The powder is weighed for standby according to the mass ratio of 99.5: 0.5. Dissolving the weighed gas atomized powder of Fe-12 wt.% Cr-2 wt.% W-0.8 wt.% Nb in 4 g.L-1The cysteine solution is soaked for 15 minutes, and then the nano La is added2O3Adding the powder into the solution, stirring for 1 hour, and drying the solution to obtain a powder precursor. And stirring the powder precursor for 2 hours in an argon atmosphere at the temperature of 500 ℃ and the rotating speed of a stirring propeller of 30000 r/min to obtain the nano-oxide coated ferrite-based alloy powder. And finally, carrying out laser cladding forming on the nano oxide coated ferrite-based alloy powder, wherein forming parameters comprise the powder laying thickness of 0.04mm, the scanning speed of 2500mm/s and the scanning distance of 0.03mm, and obtaining the ODS ferrite-based alloy product with the target shape.
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 (6)
1. A method for producing an ODS ferrite-based alloy, comprising the steps of:
s1) configuration of precursor powder: adding argon atomized FeCrWNbTi powder into a poly (diallyldimethylammonium chloride) solution or a cysteine solution, dipping, adding a rare earth-containing nano oxide source, uniformly stirring, and drying to obtain precursor powder;
the method comprises the following specific steps:
s1.1) firstly preparing a precursor solution, and then adding iron-containing gas atomized powder into the precursor solution to be soaked for 10-30 minutes to obtain a suspension solution;
s1.2) selecting a rare earth-containing nano oxide source, adding the rare earth-containing nano oxide source into the suspension solution, stirring for 0.5-6 hours, and drying the solution to obtain precursor powder;
wherein the rare earth nano oxide is used in an amount which ensures that the nano oxide in the finally prepared alloy accounts for 0.01-5wt.% of the ODS ferrite-based alloy;
the concentration of the poly (diallyldimethylammonium chloride) solution or the cysteine solution is 4-10 g.L < -1 >; the rare earth nano oxide source is Y2O3Or La2O3Powder;
the argon atomization FeCrWNbTi powder comprises the following components in percentage by weight: cr: 8-18 wt.%; w:
0.1-5 wt.%; nb: 0-2 wt.%; ti: 0-1 wt.%; the balance being Fe;
s2) heating the precursor powder obtained in the step S1) under the atmosphere protection condition to a set temperature, preserving heat, and stirring at a high speed to obtain ferrite-based alloy powder coated by nano oxides;
the method comprises the following specific steps:
s2.1) placing the obtained precursor powder in a protective atmosphere for heating to 100-600 ℃;
s2.2) preserving heat, and stirring for 0.5-4 hours by adopting a stirring propeller at the rotating speed of 15000-40000 r/min to obtain ferrite-based alloy powder coated by the nano oxide;
s3) carrying out laser cladding forming on the ferrite-based alloy powder coated with the nano-oxide obtained in S2), controlling the process to enable the metal powder to be melted by laser to form a molten pool, carrying the nano-oxide into the molten pool by the flowing of liquefied metal in the molten pool and uniformly dispersing and distributing the nano-oxide to finally obtain the ODS ferrite-based alloy with ultra-fine oxide dispersion,
the method comprises the following specific steps:
s3.1) carrying out laser cladding forming on the obtained ferrite-based alloy powder coated with the nano oxides, wherein the powder laying thickness is 0.02-0.075 mm;
s3.2) laser scanning is adopted, the scanning speed is 500-4000mm/S, the scanning distance is 0.02-0.075mm, the flow of the liquefied metal in the molten pool brings the nano-oxide into the molten pool and the nano-oxide is uniformly dispersed and distributed, and finally the ODS ferrite-based alloy with the dispersion of the ultra-fine oxide is obtained.
2. The method of claim 1, wherein the protective atmosphere is argon, nitrogen, or vacuum.
3. The method of claim 1, wherein the precursor solution concentration can be 6-8 g-L-1；
The argon atomization FeCrWNbTi powder comprises the following components in percentage by weight: 9-12 wt.% of Cr, 0.3-3 wt.% of W, 0-1.5 wt.% of Mo, 0-0.5 wt.% of Ti, and the balance of Fe;
the rare earth nano oxide is used in an amount which ensures that the nano oxide in the finally prepared alloy accounts for 0.1-1 wt% of the ODS ferrite-based alloy.
4. The method as claimed in claim 1, wherein the heating temperature in S2) can be 200-400 ℃; the rotation speed is 20000-30000 r/min, and the stirring time is 0.5-2 hours.
5. The method of claim 1, wherein in S3) the dusting thickness can be 0.03-0.05 mm; the scanning speed is 1000-2000 mm/s; the scanning distance is 0.03-0.05 mm.
6. The ODS ferrite-based alloy prepared by the method according to any one of claims 1-5, is used in the fields of the automotive industry, aerospace and nuclear industry.
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