CN114985721A - Fe-Nb-Al series Fe-based amorphous alloy powder with all metal components and preparation method thereof - Google Patents
Fe-Nb-Al series Fe-based amorphous alloy powder with all metal components and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Fe-Nb-Al series Fe-based amorphous alloy powder with all metal components and a preparation method thereof, wherein the alloy powder comprises Fe, Nb and Al; wherein, the content of each metal element is calculated by atomic percent: fe 50.0-70.0 at.%, Nb and Al in equal atomic percentage, and the total content of both is 50.0-30.0 at.%; the iron-based amorphous alloy powder has strong amorphous forming capacity, a wider supercooled liquid region and good formability, is prepared by adopting a high-energy mechanical ball milling process, is easy to control and convenient to operate, and has no strict requirements on alloy components and preparation conditions compared with the traditional quick cooling process, so that the popularization and application of the preparation method in the aspect of amorphous alloy powder preparation can be promoted.
Description
Technical Field
The invention relates to an amorphous alloy material and the processing technical field thereof, in particular to Fe-Nb-Al series iron-based amorphous alloy powder with all metal components and a preparation method thereof.
Background
The amorphous alloy has extremely high strong hardness, fracture toughness, wear resistance, excellent soft magnetic property and corrosion resistance due to the long-range disordered close packing arrangement of atoms in a three-dimensional space, so that the amorphous alloy has the potential of wide application in the fields of aerospace, precision machinery, electronic information, civil materials and the like. Among a plurality of amorphous alloy systems, the iron-based amorphous alloy has great commercial application value due to low price and excellent performance. However, the iron-based amorphous alloy has low amorphous forming ability, is only centimeter-sized, lacks room-temperature plasticity, is easy to be brittle-broken during room-temperature processing, is difficult to obtain a component with a complex shape, and greatly limits the engineering application of the component. At present, the iron-based amorphous alloy adopts the addition of metalloid elements (such as B, C, Si, P and the like) in the composition design, and improves the amorphous forming capability by forming more covalent bonds/ionic bonds in the high-purity alloy undercooled melt. However, the long-range disordered structural characteristics peculiar to amorphous alloys and the covalent/ionic bonds present inside the material make the material lack room temperature plasticity. Based on the characteristics of non-directivity and non-saturation of metal bonds, the development of the all-metal component iron-based amorphous alloy leads more metal bonds in the alloy to be beneficial to improving the room-temperature plasticity of the alloy. At present, the iron-based amorphous alloy is mostly prepared by adopting a rapid cooling process, the process has strict requirements on component proportion and preparation conditions, and the size of the material is limited by the extremely rapid cooling speed. If a powder metallurgy process is adopted, the prepared amorphous alloy powder is heated to a supercooled liquid phase region, the characteristics of viscous rheological behavior of the amorphous alloy in the supercooled liquid phase region are utilized, then the amorphous alloy is densely formed under ultrahigh pressure, and the shape and the size of the prepared bulk iron-based amorphous alloy depend on the shape and the size of a die. And the two-dimensional large-size amorphous alloy coating can also be prepared by utilizing advanced surface engineering technologies such as laser cladding, spraying and the like. The process can improve the defects of the rapid cooling process to a great extent, and achieves the aims of wider composition range and larger material size of the synthesized amorphous alloy.
At present, documents about preparing all-metal component iron-based amorphous alloy are rarely reported and are disclosed inModeling and optimization of chemical composition of nano/amorphous Fe a .Ni b .Nb c .Zr d an alloy prepared via high-energy ball milling with enhanced soft magnetic properties; in the A texture design approach document, the prepared amorphous alloy powder has nonuniform texture and nanocrystalline texture. The early stage of our topic group prepares multi-component all-metal iron-based amorphous alloy powder, and is disclosed in the title of "mechanical alloying preparation of Fe-Nb-X (X ═ Zr, Ti) pure metal component amorphous alloy" (Formation of Fe-Nb-X (X ═ Zr, Ti) amorphous from pure metals by mechanical alloying, Physica B,2012,407(2):258- 100-x (NbTiTa) x Amorphous alloy and crystallization behavior analysis "(Study of amorphous phase in Fe) 100-x (NbTiTa) x Synthesis by mechanical alloying and its effect on the crystallization phenomenon J.non-crystals solids 2014,385(1): 117-. The amorphous forming capability of Fe-Nb-X (X ═ Zr, Ti) amorphous alloy is relatively poor (the ball milling time needs 70-80 h), and Fe 100-x (NbTiTa) x The width of the supercooled liquid region of the amorphous alloy is relatively narrow (the supercooled liquid region is 101 ℃), and the amorphous alloy contains a noble metal element Ta, so that the cost is high. In addition, the two alloys are not added with a process control agent in the ball milling process, the powder is easy to stick to a pot and agglomerate, the powder yield is low, and the component structure is not uniform. The invention develops the iron-based amorphous alloy powder with all metal components, which can provide commercial raw materials for preparing large iron-based amorphous alloys with larger room temperature plasticity in powder metallurgy production due to high amorphous forming capacity and wide supercooling liquid phase region, and the commercial raw materials are inquired and not published in related patents.
Disclosure of Invention
In view of the above, the present invention aims to provide an Fe-Nb-Al based amorphous alloy powder with all metallic constituents, which has strong amorphous forming ability, a wide supercooled liquid region and good formability, and is suitable for press forming by a powder metallurgy process and for preparing an amorphous alloy coating, and a method for preparing the same.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
an all-metal component Fe-Nb-Al series iron-based amorphous alloy powder, wherein the alloy powder comprises Fe, Nb and Al; wherein, the content of each metal element is calculated by atomic percent: fe 50.0-70.0 at.%, Nb and Al in equal atomic percentage, and the total content of both is 50.0-30.0 at.%.
As a possible embodiment, further, the alloy powder is prepared by mixing Fe powder, Nb powder and Al powder, and the purity of the Fe powder, Nb powder and Al powder is higher than 99%, and the particle size is lower than 150 μm.
Based on the above, the invention also provides a preparation method of the all-metal component Fe-Nb-Al series iron-based amorphous alloy powder, which comprises the following steps:
(1) mixing Fe powder, Nb powder and Al powder according to atomic percentage, adding 2.0 wt% of stearic acid powder serving as a process control agent, and uniformly mixing a mixed system to obtain a mixed raw material;
(2) and adding the mixed raw materials into a ball mill, and carrying out ball milling processing according to preset ball milling parameters to obtain the Fe-Nb-Al series iron-based amorphous alloy powder with all metal components.
As a possible embodiment, further, in the step (1), the stearic acid powder is analytically pure, and the mixed system is dry-mixed in a V-type powder mixer until uniform.
As a possible embodiment, further, in the step (2), the mixed raw materials are ball-milled by using a QM-3SP2 type planetary high-energy ball mill to complete the preparation of the all-metallic-component Fe-Nb-Al based amorphous alloy powder; before ball milling treatment, a stainless steel ball milling tank of the ball mill is repeatedly vacuumized and filled with argon to serve as anti-oxidation protective gas.
As a possible implementation manner, further, in the step (2), the ball milling process adopts a plurality of stainless steel balls as milling balls to be mixed with the mixed raw material, wherein the diameters of the stainless steel balls are not completely the same, the diameters of the stainless steel balls respectively comprise 10mm, 5mm and 2mm, and the adding mass ratio is 2:5: 3.
As a possible embodiment, further, in the step (2), the rotating speed of the ball mill is 300r/min, the ball powder mass ratio is 20: 1; the total ball milling time is 45-55 h, the positive and negative alternate running time is 0.5h, and the alternate running interval time is 0.1h in the ball milling process.
Based on the above, the invention also provides the Fe-Nb-Al series iron-based amorphous alloy powder with the all-metal components, which is prepared by the preparation method.
As a possible implementation mode, the particle size distribution range of the all-metal component Fe-Nb-Al series iron-based amorphous alloy powder is 4-30 mu m, and the amorphous transformation temperature T of the all-metal component Fe-Nb-Al series iron-based amorphous alloy powder g And crystallization temperature T x Respectively at 578-597 ℃ and 688-690 ℃.
Based on the above, the invention also provides an amorphous alloy coating or part, which is made of the above all-metallic component Fe-Nb-Al series iron-based amorphous alloy powder.
By adopting the technical scheme, compared with the prior art, the invention has the beneficial effects that:
1. the Fe-Nb-Al series iron-based amorphous alloy powder is prepared, and the stearic acid powder as a process control agent is added, so that the prepared powder has high powder yield, short required ball milling time, uniform tissue, good fluidity due to the shape close to a sphere and wide supercooling liquid phase region, and is particularly suitable for being formed into bulk amorphous alloy through powder metallurgy process densification;
2. the amorphous alloy powder prepared by the invention has the advantages that all the constituent elements are metal elements, and all metal bonds are formed in the bulk amorphous alloy synthesized by the powder metallurgy process, so that the room temperature plasticity of the iron-based amorphous alloy material can be improved;
3. the iron-based amorphous alloy powder is prepared by adopting a high-energy mechanical ball milling process, the production process is easy to control and convenient to operate, and the requirements on alloy components and preparation conditions are not strict in the traditional quick cooling process, so that the popularization and application of the preparation method in the aspect of amorphous alloy powder preparation can be promoted.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 shows Fe prepared in example 1 60 Nb 20 Al 20 XRD patterns of the alloy powder after different ball milling times;
FIG. 2 shows Fe prepared in example 1 60 Nb 20 Al 20 SEM image of amorphous alloy powder;
FIG. 3 is Fe prepared in example 1 60 Nb 20 Al 20 A particle size distribution profile of the amorphous alloy powder material;
FIG. 4 shows Fe prepared in example 1 60 Nb 20 Al 20 DSC profile of amorphous alloy powder.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be noted that the following examples are only illustrative of the present invention, and do not limit the scope of the present invention. Similarly, the following examples are only some but not all examples of the present invention, and all other examples obtained by those skilled in the art without any inventive work are within the scope of the present invention.
Example 1
Fe 60 Nb 20 Al 20 Preparation of all-metallic constituent amorphous alloy powder
(1) Mixed powder
Firstly, high-purity Fe powder (purity: 99.8%, particle size: 48 μm), Nb powder (99.5%, 100 μm) and Al powder (99.5%, 100 μm) are mixed according to the following atomic percentage: fe 50 at.%, Nb and Al in equal atomic percentage, and the total content is 50.0-30.0 at.%, and the three elements are added in a simple substance form; then adding 2.0 wt% of stearic acid (analytically pure) powder to the metal powder, and finally dry-mixing the mixed powder in a VH-0.3V type powder mixer for 2 hours;
(2) preparation of amorphous alloy powder by high-energy ball milling
The preparation of the amorphous alloy powder is completed by adopting a QM-3SP2 planetary high-energy ball mill, the grinding balls and a ball milling tank of the ball mill are made of stainless steel materials, argon is filled into the ball milling tank after the ball milling tank is repeatedly vacuumized to prevent oxidation, the diameter of a stainless steel ball for ball milling is 10mm, the rotating speed of the ball mill is 300r/min, the mass ratio of ball powder is 20:1, and the required ball milling time is 55 h; in the ball milling process, the positive and negative alternate operation time is 0.5h, and the alternate operation interval time is 0.2 h; stopping the machine every 5h, cooling to room temperature, and sampling and analyzing.
Results and analysis of the experiments
FIG. 1 shows Fe prepared in example 1 60 Nb 20 Al 20 The XRD patterns of the alloy powder after different ball milling times show that the XRD patterns are mainly diffraction peaks of simple substance elements of the original powder when the alloy powder is not ball milled (0 h). As the ball milling time increased, the intensity of each diffraction peak gradually decreased, and part of the diffraction peaks disappeared. When the ball milling time is increased to 20h, a wider diffuse scattering peak appears in an XRD (X-ray diffraction) pattern, which indicates that the mixed powder starts to form an amorphous phase after ball milling, the diffraction peak of the Nb element disappears, and the diffraction peak of the Fe element shifts to a low diffraction angle, indicating that the Nb element with a large atomic radius is diffused and dissolved to the crystal lattice of the Fe element with a small atomic radius to form a solid solution phase in the ball milling process. When the ball milling time is prolonged to 45 hours, the diffraction peak intensity of the alloy elements is further reduced, broadened and disappeared, which shows that the mixed powder has less and less crystallization phase and is continuously converted into amorphous phase. When the ball milling is carried out for 45 hours, only broad diffuse scattering peaks exist in an XRD pattern, which indicates that the amorphous alloy powder with uniform and stable structure is successfully prepared. FIG. 2 shows Fe prepared in example 1 60 Nb 20 Al 20 In the SEM image of the amorphous alloy powder, it was found that the amorphous powder had a shape close to a spherical shape and had good powder flowability. FIG. 3 is Fe prepared in example 1 60 Nb 20 Al 20 The particle size distribution diagram of the amorphous alloy powder material shows that the particle size distribution area of the powder after ball milling is concentrated and mainly distributed between 4 and 30 mu m, and the average particle size is about 13And mu m. FIG. 4 shows Fe prepared in example 1 60 Nb 20 Al 20 DSC chart of the amorphous alloy powder, and the amorphous transition temperature T of the amorphous alloy powder can be obtained by calculating and calibrating the DSC curve g And crystallization temperature T x Respectively at 597 ℃ and 690 ℃, and the supercooling liquid phase region is as high as 93 ℃. These experimental results show that Fe 60 Nb 20 Al 20 Amorphous alloy powders are particularly suitable for forming dense bulk amorphous alloys by powder metallurgy processes.
Example 2
Fe 50 Nb 25 Al 25 Preparation of amorphous alloy powder of all-metallic constituent
This example uses a QM-3SP2 planetary ball mill as described in example 1 and the same process steps and conditions, except that the alloy components are proportioned in their atomic percentages as follows: fe 50 at.%, Nb 25 at.%, Al 25 at.%. The ball milling time is 45h, and the mixed powder is completely non-crystallized. The amorphous powder was examined for its amorphous transition temperature T g And crystallization temperature T x At 578 deg.C and 688 deg.C, respectively, and its supercooling liquid phase region is 110 deg.C.
The above description is only a part of the embodiments of the present invention, and not intended to limit the scope of the present invention, and all equivalent devices or equivalent processes performed by the contents of the present specification and the attached drawings, or directly or indirectly applied to other related technical fields, are all included in the scope of the present invention.
Claims (10)
1. An all-metal component Fe-Nb-Al series iron-based amorphous alloy powder is characterized in that the alloy powder comprises Fe, Nb and Al;
wherein, the content of each metal element is calculated by atomic percent: fe 50.0-70.0 at.%, Nb and Al in equal atomic percentage, and the total content of both is 50.0-30.0 at.%.
2. The all-metallic-component Fe-Nb-Al-based Fe-based amorphous alloy powder according to claim 1, wherein the alloy powder is made by mixing Fe powder, Nb powder and Al powder, and the purity of Fe powder, Nb powder and Al powder is higher than 99% and the particle size is lower than 150 μm.
3. A preparation method of Fe-Nb-Al series iron-based amorphous alloy powder with all metal components is characterized by comprising the following steps:
(1) mixing Fe powder, Nb powder and Al powder according to atomic percentage, adding 2.0 wt% of stearic acid powder serving as a process control agent, and uniformly mixing a mixed system to obtain a mixed raw material;
(2) and adding the mixed raw materials into a ball mill, and carrying out ball milling processing according to preset ball milling parameters to obtain the Fe-Nb-Al series iron-based amorphous alloy powder with all metal components.
4. The method for preparing an Fe-Nb-Al based amorphous alloy powder of all metallic elements according to claim 3, wherein in the step (1), the stearic acid powder is analytically pure, and the mixed system is dry-blended to be uniform in a V-type blender.
5. The method for preparing an all-metallic-component Fe-Nb-Al-based amorphous alloy powder according to claim 3, wherein in the step (2), the mixed raw materials are ball-milled by using a QM-3SP2 type planetary high-energy ball mill to complete the preparation of the all-metallic-component Fe-Nb-Al-based amorphous alloy powder;
before ball milling treatment, a stainless steel ball milling tank of the ball mill is repeatedly vacuumized and filled with argon to serve as anti-oxidation protective gas.
6. The method for preparing the all-metallic-component Fe-Nb-Al-based iron-based amorphous alloy powder according to claim 5, wherein in the step (2), a plurality of stainless steel balls with different diameters respectively including 10mm, 5mm and 2mm are mixed with the mixed raw material in a ball milling process, and the addition mass ratio is 2:5: 3.
7. The all-metallic-component Fe-Nb-Al-based iron-based amorphous alloy powder according to claim 6, wherein in the step (2), the rotation speed of the ball mill is 300r/min, and the ball powder mass ratio is 20: 1; the total ball milling time is 45-55 h, the positive and negative alternate running time is 0.5h, and the alternate running interval time is 0.1h in the ball milling process.
8. An all-metallic component Fe-Nb-Al series iron-based amorphous alloy powder, characterized in that it is obtained by the production method described in any one of claims 3 to 7.
9. The Fe-Nb-Al based amorphous alloy powder as claimed in claim 8, wherein the Fe-Nb-Al based amorphous alloy powder has a particle size distribution of 4 to 30 μm and an amorphous transition temperature T g And crystallization temperature T x Respectively at 578-597 ℃ and 688-690 ℃.
10. An amorphous alloy coating or component, characterized by: which is made of the all-metallic component Fe-Nb-Al based amorphous alloy powder of claim 8 or 9.
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