CN114985749A - Oxide-amorphous composite powder for ODS-W alloy and preparation method thereof - Google Patents
Oxide-amorphous composite powder for ODS-W alloy and preparation method thereof Download PDFInfo
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Abstract
An oxide-amorphous composite powder for ODS-W alloy and a preparation method thereof, belonging to the field of powder preparation engineering. The powder material is characterized in that nano-scale spherical oxide particles with different number densities are dispersed on an amorphous alloy matrix, and the chemical composition of the oxide-amorphous composite powder is G + (3-40 wt%) Y 2 O 3 Wherein G ═ Y a X 100‑a Y is yttrium, and X is Fe, Co or Ni. The invention firstly needs to obtain alloy melt with nano oxide particles uniformly distributed therein by induction melting, and obtains oxide-amorphous composite powder materials with different particle diameters by a melt atomization technology. The invention successfully implements oxygenKilogram-level manufacture of compound-amorphous composite powder realizes large-scale preparation; powder materials with different oxide contents can be obtained by regulating and controlling the content ratio of the amorphous matrix to the nano oxide, and the oxide-amorphous composite powder with ultrahigh oxide content is successfully prepared; the alloy system and the component range of the powder amorphous matrix are widened, and the preparation efficiency is high.
Description
Technical Field
The invention belongs to the field of powder preparation engineering, and relates to an oxide-amorphous composite powder material and a preparation method thereof.
Background
By introducing uniform and dispersed nano oxide particle reinforcement into a metal or alloy matrix, the ODS alloy which is a composite material with excellent comprehensive physical property and mechanical property is expected to be developed. The dispersion-strengthened phase of ODS-tungsten (W) alloy is an oxide (e.g. Y) having high thermal and chemical stability 2 O 3 ) Or particles of a ceramic phase (SiC, etc.). The ODS-W alloy has the structural characteristics that: the micro-nano-sized strengthening phase particles are uniformly and dispersedly distributed in W crystalIntra-granular and at grain boundaries. The advanced W alloy has extremely high melting point, high thermal conductivity, excellent high-temperature creep resistance, high recrystallization temperature and physical sputtering and hot corrosion resistance, and has wide application prospect in the fields of nuclear reactors, aerospace and other energy sources, carrying engineering and the like.
Mechanical Alloying (MA) is currently the most common and efficient method for preparing ODS-W alloys. The method comprises the steps of mixing W and oxide powder, performing ball milling, and sintering to form. Wherein, ball milling powder preparation is a key link for determining the structure and performance of ODS-W alloy. The main problems of the MA method for preparing the sintering precursor powder are that: impurities are inevitably introduced in the ball milling process to pollute a sample, oxides at the grain boundary in a sintered body are easy to agglomerate, and the sintering quality of the ODS-W alloy is seriously damaged.
Researchers have tried various methods to improve and solve the problems of oxide segregation and impurities in the preparation process of ODS-W alloy. For example, Ni-coated Y is obtained by electroless Ni plating 2 O 3 Powder; preparation of W-coated Y by hydrothermal method 2 O 3 Nanopowders, and the like. In order to improve the binding force between the particles and the coating layers, the preparation of the coating oxides needs to be carried out on Y in advance 2 O 3 The nano particles are subjected to surface modification treatment, so that the agglomeration of the nano oxide powder is easily initiated. Therefore, the crystalline metal coating method has little effect on solving the problem of segregation of the nano-oxide. Recently, amorphous coating treatment of oxide particles has been proposed to improve the agglomeration problem of nano-oxide during the preparation of ODS-W alloy (CN112831733A), and to improve the dispersion and strengthening effect of oxide particles in ODS-W alloy. However, the preparation and application of the amorphous coated oxide powder particles at present have many defects. We notice that the existing amorphous coating oxide particle powder preparation method combining melt-spun and ball milling is not only limited by the amorphous forming capability of matrix alloy and the compatibility of an amorphous matrix and an oxide, but also has the problems of multi-parameter control and balance in the preparation process. These seriously affect the quality and yield of the amorphous coated oxide particles, and are difficult to meet the requirement of mass preparation of ODS-W alloy. Meanwhile, the melt-spun rapid quenching technology is difficult to obtain the product with high oxygen contentCrystalline alloy and amorphous coated powder with high oxide content (CA 110129609A). These problems are not favorable for the industrial production and practical use of the novel ODS-W alloy.
Disclosure of Invention
The invention aims to solve the problems that: overcomes and improves the defects existing in the prior preparation of oxide-amorphous composite powder materials that (1) the oxygen content of the intermediate alloy is low, and the amorphous matrix alloy system and components are narrow; (2) the difficulty in parameter matching and control of the single-roller melt-spinning-ball milling process is high, the repeatability and controllability of powder (such as particle size and shape) are poor, and amorphous coated powder with high oxide content is difficult to obtain; and (3) the problems of low milling efficiency, high cost, unsuitability for large-scale production and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
the oxide-amorphous composite powder based on the melt atomization technology is characterized in that nanoscale spherical oxide particles with different numbers and densities are dispersed and distributed on an amorphous alloy matrix, and the chemical composition of the oxide-amorphous composite powder is G + (3-40 wt%) Y% 2 O 3 Wherein G ═ Y a X 100-a Is an atomic percentage composition of amorphous matrix alloy, Y is rare earth metal yttrium, X is Fe, Co or Ni metal, and the oxide particles are Y 2 O 3 . The invention firstly needs to obtain the (amorphous component) alloy melt in which the nano oxide particles are uniformly distributed by induction melting. Where G-Y is required a X 100-a Amorphous matrix melt and oxide Y 2 O 3 The particles have good chemical affinity and wettability, and the density of the particles is similar to that of the particles, so that gravity segregation and oxide particle segregation are avoided. On the basis, the oxide-amorphous composite powder materials with different grain diameters are obtained by a melt atomization technology.
A method for preparing oxide-amorphous composite powder based on a melt atomization technology comprises the following steps:
(1) firstly, preparing and smelting a kilogram-level amorphous matrix alloy ingot with a G component;
the component G ═ Y a X 100-a A is atomic percent, the value of a is more than or equal to 30 and less than or equal to 85, the rare earth metal Y and X are contained, X is one or more of Fe, Co or Ni elements, and Y is rare earth metal yttrium; mixing the prepared industrial pure metal raw materials, placing the mixture in a crucible of a medium-frequency induction smelting furnace, vacuumizing to 1-10 Pa, filling 0.01-0.10 MPa of industrial pure Ar protective gas, electrifying to carry out induction smelting, wherein the smelting temperature and the smelting time are 800-1300 ℃ respectively, and 5-10 min, and finally obtaining a kilogram-level uniform alloy ingot with the component of G.
(2) Secondly, preparing and smelting kilogram-grade G + (3-40 wt%) Y 2 O 3 Alloy, obtaining oxide-amorphous composite powder
2.1) determining Y in the oxide-amorphous composite powder according to the size and distribution of the actually required oxide reinforcement prepared from ODS-W alloy 2 O 3 The addition amount and the specific components.
2.2) crushing the G alloy ingot obtained in the first step, and weighing Y according to the proportion obtained in the step 2.1) 2 O 3 Mixing nano oxide and G alloy material to prepare kilogram-level oxide-amorphous composite material, wherein Y is 2 O 3 The weight ratio of the nano oxide can be 3-40 wt%, and the corresponding general formula of the oxide-amorphous composite alloy can be expressed as G + (3-40 wt%) Y 2 O 3 . Here, G ═ Y a X 100-a Matrix melt and oxide Y 2 O 3 The particles have good chemical affinity and wettability, and the density of the particles is similar to that of the particles, so that gravity segregation and oxide particle segregation can be avoided.
2.3) mixing the prepared kilogram-grade G + (3-40 wt%) Y 2 O 3 Placing the alloy material in an atomizing furnace crucible, and heating to a certain temperature (800-1300 ℃, wherein the temperature is required to be higher than the melting point of G alloy and far lower than Y alloy) 2 O 3 Melting point of oxide), keeping the temperature for 2-5min to obtain an alloy melt with G as a component, wherein oxide particles are uniformly distributed in the alloy melt; then atomizing and spraying the mixture for cooling (the spraying pressure of atomizing gas is 5-10 MPa, the aperture of a nozzle of a guide rod is 2-7 mm) to obtain a spherical powder material, wherein the particle size of the spherical powder material is controllable and can be changed within 5-300 mu m.
(3) And thirdly, adopting a scanning electron microscope, and representing the powder form and structure by combining an X-ray diffractometer and an electron microscope technology. The results show that: the matrix of the obtained spherical powder is amorphous alloy with the component of G, wherein nanometer-scale oxide particles are uniformly and dispersedly distributed to form the oxide-amorphous composite material.
The invention has the beneficial effects that:
(1) the invention successfully implements kilogram-level manufacture of the oxide-amorphous composite powder and can realize large-scale preparation of related powder materials;
(2) powder materials with different oxide contents (1-40 wt%) can be obtained by regulating and controlling the content ratio of the amorphous matrix to the nano oxide, and the preparation of the oxide-amorphous composite powder with ultrahigh oxide content (40 wt%) is realized;
(3) the alloy system and component range of the amorphous matrix of the oxide-amorphous composite powder can be remarkably widened, and the oxide-amorphous composite powder can be widely applied to most amorphous alloy forming systems and components;
(4) meanwhile, the atomization technology can obviously improve the preparation efficiency of the material, and the preparation of kilogram-level oxide-amorphous composite powder materials with different particle sizes can be conveniently realized through the regulation and control of atomization process parameters.
Drawings
FIG. 1 shows Y in example 1 2 O 3 -Y 70 Fe 30 Spherical appearance (scanning electron microscope secondary electron image) of the amorphous composite powder.
FIG. 2 shows Y in example 1 2 O 3 -Y 70 Fe 30 X-ray diffraction pattern of amorphous composite powder.
FIG. 3 shows Y in example 1 2 O 3 -Y 70 Fe 30 Amorphous composite powder TEM microstructure (bright field image and Y) 2 O 3 Particle diffraction spectrum).
Detailed Description
The oxide-amorphous composite powder and the embodiments thereof according to the present invention will be described in detail below. The concrete preparation process and application of the material and the powder thereof are described by taking five typical components as examples.
Example 1Y 70 Fe 30 +5wt％Y 2 O 3 Oxide-amorphous composite powder
Step one, preparing Y by induction melting 70 Fe 30 Alloy ingot (5 kg):
the method comprises the steps of weighing and preparing an atomic percentage component of Y by taking industrial pure Y (more than 99.5%) and Fe (more than 99.5%) as raw materials 70 Fe 30 The alloy of (1). Placing the alloy raw material in a crucible of an induction smelting furnace, vacuumizing to 10Pa, filling 0.07MPa of industrial pure Ar gas for protection, carrying out induction smelting at the smelting temperature of 900 ℃ for 8min, and finally obtaining Y with uniform components 70 Fe 30 And (3) alloy ingots.
Step two, atomizing to prepare Y 70 Fe 30 +5wt％Y 2 O 3 Oxide-amorphous composite powder (5kg)
Firstly, Y is 70 Fe 30 Crushing the alloy ingot, mixing with purchased Y 2 O 3 Nano oxide as raw material according to Y 70 Fe 30 +5wt％Y 2 O 3 Weighing and preparing 5kg of alloy according to the component ratio, mixing the alloy and the alloy, placing the mixture into a crucible of an atomizing furnace, heating the mixture to 900 ℃, keeping the temperature for 3min, then spraying and atomizing the mixture, wherein the spraying pressure of atomizing gas is 10MPa, the aperture of a nozzle of a guide rod is 5mm, and cooling the mixture to obtain alloy powder.
Scanning electron microscopy observations showed (fig. 1): the shape of the powder sample is spherical, and the particle size of most of the powder is 50-100 mu m; XRD analysis (fig. 2) showed: the powder sample has typical amorphous structure diffuse package characteristics, and cI80-Y is distributed on the powder sample 2 O 3 Sharp diffraction peaks of the crystalline phase; FIG. 3 shows the TEM analysis of the powder sample, from which the nanoscale Y is visible 2 O 3 The oxide particles are uniformly and dispersedly distributed in the amorphous matrix, and the tissue uniformity of the whole sample is good.
Example 2Y 65 Co 30 Ni 5 +10wt％Y 2 O 3 Oxide-amorphous composite powder
Step one, preparing Y by induction melting 65 Co 30 Ni 5 Alloy ingot (1)0kg)：
The industrial pure Y (more than 99.5 percent), Co (more than 99.5 percent) and Ni (more than 99.5 percent) are adopted as raw materials, and Y is weighed and prepared as the atomic percentage component 65 Co 30 Ni 5 The alloy of (1). Placing alloy raw materials in a crucible of an induction smelting furnace, vacuumizing to 6Pa, filling 0.05MPa of industrial pure Ar gas for protection, carrying out induction smelting at the smelting temperature of 800 ℃ for 8min, and finally obtaining Y with uniform components 65 Co 30 Ni 5 And (3) alloy ingot.
Step two, atomizing to prepare Y 65 Co 30 Ni 5 +10wt％Y 2 O 3 Oxide-amorphous composite powder (10kg)
Firstly, Y is 65 Co 30 Ni 5 Crushing the alloy ingot, mixing with the purchased Y 2 O 3 Nano oxide as raw material according to Y 65 Co 30 Ni 5 +10 wt％Y 2 O 3 Weighing and preparing 10kg of alloy according to the component ratio, mixing the alloy and the alloy, placing the mixture in a crucible of an atomizing furnace, heating to 800 ℃, keeping the temperature for 2min, then spraying and atomizing, wherein the spraying pressure of atomizing gas is 5MPa, the aperture of a nozzle of a guide rod is 2mm, and cooling to obtain alloy powder.
And (3) adopting a scanning electron microscope, and combining an X-ray diffractometer and an electron microscope technology to represent the powder form and structure. The results show that: the matrix of the obtained spherical powder is Y 65 Co 30 Ni 5 In which nano-scale Y is uniformly and dispersedly distributed 2 O 3 Oxide particles, the sample overall texture uniformity is good. The particle size of the powder of the oxide-amorphous composite material is 5-15 mu m, and the average particle size is 10 mu m.
Example 3Y 30 Co 70 +3wt％Y 2 O 3 Oxide-amorphous composite powder material
Step one, preparing Y by induction melting 30 Co 70 Alloy ingot (10 kg):
the industrial pure Y (more than 99.5 percent) and Co (more than 99.5 percent) are adopted as raw materials, and the component with atomic percentage of Y is weighed and prepared 30 Co 70 The alloy of (1). The alloy raw material is placed in induction meltingVacuumizing the furnace crucible to 1Pa, introducing 0.01MPa of industrial pure Ar gas for protection, and carrying out induction melting at 1300 ℃ for 10min to finally obtain Y with uniform components 30 Co 70 And (3) alloy ingot.
Step two, atomizing to prepare Y 30 Co 70 +3wt％Y 2 O 3 Oxide-amorphous composite powder (10kg)
Firstly, Y is 30 Co 70 Crushing the alloy ingot, mixing with purchased Y 2 O 3 Nano oxide as raw material according to Y 30 Co 70 +3wt％Y 2 O 3 Weighing and preparing 10kg of alloy according to the component ratio, mixing the alloy and the alloy, placing the mixture in an atomizing furnace crucible, heating to 1300 ℃, keeping the temperature for 3min, then spraying and atomizing, wherein the spraying pressure of atomizing gas is 10MPa, the aperture of a nozzle of a guide rod is 5mm, and cooling to obtain alloy powder.
And (3) adopting a scanning electron microscope, and combining an X-ray diffractometer and an electron microscope technology to represent the powder form and structure. The results show that: the matrix of the obtained spherical powder is Y 30 Co 70 In which nano-scale Y is uniformly and dispersedly distributed 2 O 3 Oxide particles, the sample overall texture uniformity is good. The particle size of the powder of the oxide-amorphous composite material is 50-100 mu m, and the average particle size is 80 mu m.
Example 4Y 85 Fe 15 +40wt％Y 2 O 3 Oxide-amorphous composite powder
Step one, preparing Y by induction melting 85 Fe 15 Alloy ingot (5 kg):
the method comprises the steps of weighing and preparing an atomic percentage component of Y by taking industrial pure Y (more than 99.5%) and Fe (more than 99.5%) as raw materials 85 Fe 15 The alloy of (1). Placing alloy raw materials in a crucible of an induction smelting furnace, vacuumizing to 10Pa, filling 0.10MPa of industrial pure Ar gas for protection, carrying out induction smelting at the smelting temperature of 1150 ℃ for 6min, and finally obtaining Y with uniform components 85 Fe 15 And (3) alloy ingots.
Step two, atomizing to prepare Y 85 Fe 15 +40wt％Y 2 O 3 Oxide-amorphous composite powder (5kg)
Firstly, Y is 85 Fe 15 Crushing the alloy ingot, mixing with the purchased Y 2 O 3 Nano oxide as raw material, according to Y 85 Fe 15 +40wt％Y 2 O 3 Weighing and preparing 5kg of alloy according to the component ratio, mixing the alloy and the alloy, placing the mixture in an atomizing furnace crucible, heating to 1150 ℃, keeping the temperature for 5min, then spraying and atomizing, wherein the spraying pressure of atomizing gas is 10MPa, the aperture of a nozzle of a guide rod is 7mm, and cooling to obtain alloy powder.
The powder form and structure are represented by adopting a scanning electron microscope and combining an X-ray diffractometer and an electron microscope technology. The results show that: the obtained spherical powder has a matrix with a component of Y 85 Fe 15 In which nano-scale Y is uniformly and dispersedly distributed 2 O 3 Oxide particles, the sample overall texture homogeneity is good. The particle size of the powder of the oxide-amorphous composite material is 150-300 mu m, and the average particle size is 200 mu m.
Example 5Y 75 Ni 25 +10wt％Y 2 O 3 Oxide-amorphous composite powder
Step one, preparing Y by induction melting 75 Ni 25 Alloy ingot (5 kg):
the industrial pure Y (more than 99.5 percent) and Ni (more than 99.5 percent) metals are used as raw materials, and the component with atomic percentage of Y is weighed and prepared 75 Ni 25 The alloy of (1). Placing alloy raw materials in a crucible of an induction smelting furnace, vacuumizing to 5Pa, filling 0.05MPa of industrial pure Ar gas for protection, carrying out induction smelting at the smelting temperature of 900 ℃ for 6min, and finally obtaining Y with uniform components 75 Ni 25 And (3) alloy ingots.
Step two, atomizing to prepare Y 75 Ni 25 +10wt％Y 2 O 3 Oxide-amorphous composite powder (5kg)
Firstly, Y is 75 Ni 25 Crushing the alloy ingot, mixing with the purchased Y 2 O 3 Nano oxide as raw material according to Y 75 Ni 25 +10wt％Y 2 O 3 Weighing the components, preparing 5kg of alloy, mixing the componentsPlacing in an atomizing furnace crucible, heating to 900 ℃, keeping the temperature for 3min, then spraying and atomizing, wherein the spraying pressure of atomizing gas is 5MPa, the aperture of a nozzle of a guide rod is 3mm, and cooling to obtain alloy powder.
And (3) adopting a scanning electron microscope, and combining an X-ray diffractometer and an electron microscope technology to represent the powder form and structure. The results show that: the matrix of the obtained spherical powder is Y 75 Ni 25 In which nano-scale Y is uniformly and dispersedly distributed 2 O 3 Oxide particles, the sample overall texture uniformity is good. The particle size of the powder of the oxide-amorphous composite material is 30-70 mu m, and the average particle size is 50 mu m.
In order to reveal and verify the beneficial effects of the oxide-amorphous composite powder material provided by the invention, the oxide-amorphous composite powder material is used as a reinforcing phase to prepare the ODS-W alloy. Specifically, the alloy powder prepared in the third step of example 1 and tungsten powder are weighed and mixed according to the weight ratio of 1:50, and the mixture is placed in a planetary ball mill to be mechanically and uniformly mixed; then, preparing an ODS-W alloy sintered body by a hot pressing body sintering technology, wherein the sintering temperature is 1750 ℃, the temperature is kept for 3 hours, an amorphous matrix of oxide particles is melted in the sintering process, a compact and good chemical bonding interface is formed through the flow and filling of related liquid phases and the fusion of a matrix tungsten and an oxide nanoparticle reinforcing phase in the amorphous matrix (similar to a brazing process), and finally the sintering density of the ODS-W alloy can reach more than 98%.
For the current Y 2 O 3 Enhancement of Y present during preparation of ODS alloy 2 O 3 The method for preparing the oxide-amorphous composite powder material by the atomization technology can obviously improve the content of the oxide in the material and broaden the amorphous matrix alloy system and components; the problems of high parameter matching and control difficulty, poor controllability and high product control fluctuation of a single-roller melt-spinning-ball milling process are avoided; simplifies the process steps, improves the powder preparation efficiency and is suitable for large-scale industrial production.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (7)
1. A method for preparing oxide-amorphous composite powder based on a melt atomization technology is characterized by comprising the following steps:
(1) preparing and smelting a kilogram-level amorphous matrix alloy ingot with a G component;
the component G ═ Y a X 100-a A is atomic percent, is not less than 30 and not more than 85, and comprises rare earth metals Y and X, wherein X is a metal element, and Y is rare earth metal yttrium; mixing the prepared industrial pure metal raw materials, placing the mixture into a crucible of a medium-frequency induction smelting furnace, vacuumizing, filling industrial pure Ar protective gas, and electrifying to carry out induction smelting to obtain a kilogram-level uniform alloy ingot with the component of G;
(2) preparing and smelting kilogram-grade G + (3-40 wt%) Y 2 O 3 Alloy, obtaining oxide-amorphous composite powder
2.1) determining Y in the oxide-amorphous composite powder according to the actually required size and distribution of the oxide reinforcement prepared from the ODS-W alloy 2 O 3 The addition amount and specific components;
2.2) crushing the G alloy ingot obtained in the first step, and weighing Y according to the proportion obtained in the step 2.1) 2 O 3 Mixing nano oxide and G alloy material to prepare kilogram-level oxide-amorphous composite material, wherein Y is 2 O 3 The weight ratio of the nano oxide is 3-40 wt%, and the corresponding general formula of the oxide-amorphous composite alloy can be expressed as G + (3-40 wt%) Y 2 O 3 (ii) a Where G is Y a X 100-a Matrix melt and oxide Y 2 O 3 The particles have good chemical affinity and wettability, and the density of the particles is close to that of the particles, so that gravity segregation and oxide particle segregation can be avoided;
2.3) mixing the prepared kilogram-grade G + (3-40 wt%) Y 2 O 3 Placing the alloy material in a crucible of an atomizing furnace, heating to a certain temperature, and then preserving heat, wherein the temperature is higher than the melting point of G alloy and lower than Y 2 O 3 Melting point of oxide to obtain alloy melt with G component and oxide grains distributed homogeneously; then atomizing, spraying and cooling the mixture to obtain the spherical powder material, wherein the particle diameter of the spherical powder material is controllable and can be changed between 5 and 300 mu m.
2. The method for preparing the oxide-amorphous composite powder based on the melt atomization technology as claimed in claim 1, wherein in the step (1), the metal element X is one or more of Fe, Co or Ni.
3. The method for preparing the oxide-amorphous composite powder based on the melt atomization technology as claimed in claim 1, wherein in the step (1), the vacuum is pumped to 1-10 Pa, and industrial pure Ar protective gas of 0.01-0.10 MPa is filled.
4. The method for preparing the oxide-amorphous composite powder based on the melt atomization technology as claimed in claim 1, wherein in the step (1), the induction melting temperature and the induction melting time are 800-1300 ℃ and 5-10 min respectively.
5. The method for preparing the oxide-amorphous composite powder based on the melt atomization technology as claimed in claim 1, wherein in the step (2.3), the heating temperature is 800-1300 ℃, and the holding time is 2-5 min.
6. The method for preparing the oxide-amorphous composite powder based on the melt atomization technology as claimed in claim 1, wherein in the atomization, ejection and cooling processes in the step (2.3), the atomization gas ejection pressure is 5-10 MPa, and the nozzle aperture of the guide rod is 2-7 mm.
7. The oxide-amorphous composite powder based on the melt atomization technology, which is obtained by the preparation method of any one of claims 1 to 6, is characterized in that the matrix of the obtained spherical powder is amorphous alloy with the component G, and nano-scale oxide particles are uniformly and dispersedly distributed in the amorphous alloy to form the oxide-amorphous composite material.
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