CN111334682A - Nano porous metal powder and preparation method thereof - Google Patents
Nano porous metal powder and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
- C22C3/005—Separation of the constituents of alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
Abstract
The invention relates to a nano porous metal powder and a preparation method thereof. To facilitate separation of the primary phase, the first alloy is reheated and the first matrix phase is remelted and solidified into an amorphous second matrix phase by controlling the heating temperature and the second solidification rate, resulting in a second alloy. And finally, preparing the nano porous metal powder of the flaky hexagonal particles by an alloy removing method, wherein the nano porous metal powder is of a nano porous structure. The preparation method provided by the invention is simple in process, and the obtained nano-porous metal powder is large in specific surface area, and has excellent properties such as good particle fluidity, high thermal conductivity, high electrical conductivity and corrosion resistance, so that the nano-porous metal powder has important application in the fields of catalysis, new energy, photoelectricity and the like.
Description
RELATED APPLICATIONS
The priority of the chinese patent application, entitled "metallic material and method for making the same", filed on 12.3.2020, 202010170802.2, is hereby incorporated by reference in its entirety.
Technical Field
The invention relates to the technical field of nano porous metal powder, in particular to nano porous metal powder and a preparation method thereof.
Background
At present, the preparation method of the nano porous metal powder is mainly an alloy removing method. According to the method, the nano porous metal powder is prepared by corroding relatively active elements in the alloy and constructing a three-dimensional porous three-dimensional structure through diffusion rearrangement of surplus inert elements. In general, the dealloying method is suitable for preparing large-sized block or strip nano-porous materials; or the nano porous powder material is further prepared by crushing the precursor alloy into powder. However, the nanoporous powder particles obtained by these methods are generally of arbitrary shape and it is difficult to precisely control the morphology thereof.
Disclosure of Invention
In view of the above, there is a need to provide a nanoporous metal powder and a method for preparing the same; the preparation method can obtain the nano-porous metal powder of flaky hexagonal particles.
A method of making a nanoporous metal powder comprising:
according to the formula MgaCubMcREdWeighing the raw materials, wherein,m is selected from at least one of Au, Pt, Pd, Ru, Rh and Ir, RE is at least one of rare earth elements, a, b, c and d respectively represent the atomic percentage content of each element, 55 percent to 70 percent of a, 15 percent to 25 percent of b, 2 percent to 10 percent of c and a + b + c + d are 100 percent, the raw materials are melted and then cooled to room temperature at a first solidification rate to obtain a first alloy, wherein the solidification structure of the first alloy comprises a primary crystal phase rich in M and at least one of Cu and RE, the primary crystal phase is in a shape of a sheet hexagon and has a melting point T of TmThe melting point of the first matrix phase is Tn，Tn<Tm；
Heating the first alloy to a temperature T, and then cooling to room temperature at a second solidification rate, the second solidification rate being greater than the first solidification rate, to obtain a second alloy, wherein T isn<T<TmThe second alloy comprises an amorphous second matrix phase and the primary crystal phase distributed in the second matrix phase;
and providing an acid solution, mixing the second alloy with the acid solution, reacting the second matrix phase with the acid solution to obtain ions which enter the solution, separating the primary crystal phase out and reacting with the acid solution to obtain the nano-porous metal powder with the component M, wherein the nano-porous metal powder is sheet-shaped hexagonal particles and has a nano-porous structure.
In one embodiment, the first solidification rate is 0.1K/s to 500K/s, and the second solidification rate is 103K/s～107K/s。
In one embodiment, the TnAt 460 to 495 ℃, said TmIs 510 ℃ to 555 ℃.
In one embodiment, the thickness of the primary crystal phase is 50nm to 1000 nm.
In one embodiment, the primary crystal phase is in the shape of a regular hexagon in a sheet shape.
In one embodiment, the diameter of the circumcircle of the regular hexagon is 1-10 μm.
In one embodiment, the acid in the acid solution is at least one of hydrochloric acid, nitric acid and sulfuric acid, and the molar concentration of the acid in the acid solution is 1mol/L to 10 mol/L.
In one embodiment, the temperature for mixing the second alloy and the acid solution is 0-100 ℃, and the reaction time is 10 min-3 h.
In one embodiment, the size of the porous ligaments in the nanoporous structure is between 20nm and 100 nm.
The preparation method of the nano-porous metal powder comprises the following steps of preparing a nano-porous metal powder, wherein the nano-porous metal powder comprises the following components of M, wherein M is at least one selected from Au, Pt, Pd, Ru, Rh and Ir, the nano-porous metal powder is in the shape of flaky hexagonal particles, and the nano-porous metal powder is in a nano-porous structure.
In the preparation method of the present invention, first, a specific component is selected to be melted into a melt, and the first alloy obtained by solidification has a primary crystal phase in a sheet-like hexagonal shape and a first matrix phase by controlling a first solidification rate. To facilitate separation of the primary phase, the first alloy is reheated and the first matrix phase is remelted and solidified into an amorphous second matrix phase by controlling the heating temperature and the second solidification rate, resulting in a second alloy. And finally, preparing the nano porous metal powder of the flaky hexagonal particles by an alloy removing method, wherein the nano porous metal powder is of a nano porous structure, and the method is simple, low in cost and free of impurities.
In addition, the size and shape of the resulting nanoporous metal powder substantially correspond to the size and shape of the primary crystalline phase in the first alloy. Therefore, in order to obtain the nanoporous metal powder having a suitable size and shape, the size and shape of the primary crystal phase in the first alloy may be controlled by controlling the first solidification rate, and specifically, the higher the first solidification rate is, the thinner the thickness of the sheet-shaped hexagonal primary crystal phase is, and the smaller the circumscribed circle diameter is.
Therefore, the nano-porous metal powder has a hexagonal flaky shape and a nano-porous structure, has a large specific surface area, and also has excellent properties such as good particle fluidity, high thermal conductivity, high electrical conductivity, corrosion resistance and the like, so that the nano-porous metal powder has important applications in the fields of catalysis, new energy, photoelectricity and the like, and particularly has a very good application prospect in the fields (such as catalysis and the like) with requirements on the shape of the nano-porous metal powder.
Drawings
FIG. 1 is a fracture SEM photograph of a second alloy prepared according to example 1 of the present invention;
FIG. 2 is a SEM photograph of an Au material prepared in example 1 of the present invention;
FIG. 3 is a side SEM photograph of an Au material prepared in example 1 of the present invention;
FIG. 4 is an energy spectrum of Au material prepared in example 1 of the present invention.
Detailed Description
The nanoporous metal powder and the method for preparing the same according to the present invention will be further described below.
The preparation method of the nano-porous metal powder provided by the invention comprises the following steps:
s1, Mg according to the formulaaCubMcREdWeighing raw materials, wherein M is selected from at least one of Au, Pt, Pd, Ru, Rh and Ir, RE is at least one of rare earth elements, a, b, c and d respectively represent the atomic percentage content of each element, 55% to 70% of a, 15% to 25% of b, 2% to 10% of c and 100% of a + b + c + d, melting the raw materials, cooling to room temperature at a first solidification rate to obtain a first alloy, wherein the solidification structure of the first alloy comprises an M-rich primary crystal phase and a first matrix phase, the primary crystal phase comprises M and at least one of Cu and RE, the shape of the primary crystal phase is a sheet hexagon, and the melting point of the primary crystal phase is TmThe melting point of the first matrix phase is Tn，Tn<Tm；
S2, heating the first alloy to a temperature T, and then cooling to room temperature at a second solidification rate, wherein the second solidification rate is greater than the first solidification rate, to obtain a second alloy, wherein Tn<T<TmThe second alloy comprises an amorphous second matrix phase and the primary crystal phase distributed in the second matrix phase;
and S3, providing an acid solution, mixing the second alloy with the acid solution, reacting the second matrix phase with the acid solution to obtain ions which enter the solution, separating the primary crystal phase and reacting with the acid solution to obtain the nano-porous metal powder with the component M, wherein the nano-porous metal powder is sheet hexagonal particles and has a nano-porous structure.
In step S1, the molecular formula of Mg can be directly providedaCubMcREdThe precursor alloy can also be prepared by metal Mg, metal Cu, metal M and rare earth RE and smelted into the precursor alloy with the formula of MgaCubMcREdThe precursor alloy of (1).
In the process of melting and solidifying the raw materials into the first alloy, the primary crystal phases formed by the metals M, Cu and RE are firstly separated out through the regulation and control of the first solidification rate, and the melting point of the primary crystal phases is Tm，TmIs 510 ℃ to 555 ℃. The primary crystal phase is flaky hexagon, and moreover, the size of the primary crystal phase can be controlled through regulating and controlling the first solidification rate, and specifically, the higher the first solidification rate is, the thinner the thickness of the flaky hexagonal primary crystal phase is, and the smaller the circumscribed circle diameter is. However, if the first solidification rate is too high, precipitation of the primary crystal phase is suppressed, resulting in incomplete precipitation thereof. Therefore, the first solidification rate is 0.1K/s to 500K/s.
Further, the thickness of the obtained primary crystal phase is 50nm to 1000nm, the shape of the primary crystal phase is a sheet-shaped regular hexagon, and the diameter of a circumscribed circle of the regular hexagon is 1 μm to 10 μm.
In addition, in the process of melting and solidifying the raw materials into the first alloy, the remaining Mg, Cu, and RE having amorphous forming ability are solidified into the first matrix phase having a melting point Tn，TnAt 460-495 ℃ Tn<Tm。
It should be noted that the first matrix phase may comprise, in addition to the eutectic structure, other complex crystalline phases with significantly different compositions, which are detrimental to the homogeneous reaction of dealloying and the subsequent separation from the primary crystalline phase.
Therefore, in step S2, the present invention re-heats the first alloy to the temperature range T, Tn<T<TmSo that the first matrix phase is melted and the primary crystal phase is not melted, and a semi-solid alloy melt is obtained. And cooling the semi-solid alloy melt to room temperature at a second solidification rate to obtain an amorphous second matrix phase, and distributing a primary crystal phase in the amorphous second matrix phase to obtain a second alloy. The second alloy is preferably a thin strip, the thickness of which is preferably 10 μm to 500 μm.
Specifically, the second solidification rate is 103K/s～107K/s。
It will be appreciated that the average molecular formula of the first and second alloys is still MgaCubMcREd。
In step S3, the second matrix phase in the second alloy reacts with an acid by using a dealloying method to become an ion entering solution, and the primary crystal phase is separated. Since the primary crystal phase also contains at least one of Cu and RE, the separated primary crystal phase reacts with an acid to further remove elements other than M, thereby obtaining a nanoporous metal powder having a nanoporous structure as component M.
Specifically, the size of the frenulum in the nano porous structure is 20 nm-100 nm.
Specifically, the acid in the acid solution is at least one of hydrochloric acid, nitric acid and sulfuric acid, the molar concentration of the acid in the acid solution is 1-10 mol/L, the mixing temperature of the second alloy and the acid solution is 0-100 ℃, and the reaction time is 10 min-3 h.
Therefore, the present invention also provides a nanoporous metal powder prepared by the above preparation method, wherein the component of the nanoporous metal powder is M, M is at least one selected from Au, Pt, Pd, Ru, Rh, and Ir, the shape of the nanoporous metal powder is a sheet-like hexagonal particle, and the nanoporous metal powder has a nanoporous structure.
Specifically, the thickness of the nano-porous metal powder is 50 nm-1000 nm, the nano-porous metal powder is in a regular hexagon sheet shape, the diameter of a circumscribed circle of the regular hexagon is 1 μm-10 μm, and the size of a frenulum in the nano-porous structure is 20 nm-100 nm.
Therefore, the nano-porous metal powder has a hexagonal flaky shape and a nano-porous structure, has a large specific surface area, and also has excellent properties such as good particle fluidity, high thermal conductivity, high electrical conductivity, corrosion resistance and the like, so that the nano-porous metal powder has important applications in the fields of catalysis, new energy, photoelectricity and the like, and particularly has a very good application prospect in the fields (such as catalysis and the like) with requirements on the shape of the nano-porous metal powder.
Hereinafter, the nanoporous metal powder and the method for preparing the same will be further described by the following specific examples.
Example 1
Selected component is Mg61Cu23Au5Gd11The precursor alloy is prepared into alloy according to the element composition, the alloy is fully melted by induction, and then the alloy melt is solidified to room temperature at the speed of 50K/s to obtain the precursor alloy with the component of Mg61Cu23Au5Gd11The first alloy of (1). In the solidification process, an Au-rich primary crystal phase with the element composition of Au-Cu-Gd is firstly precipitated, and the residual melt with amorphous forming capability is solidified into a first matrix phase, wherein the melting point of the primary crystal phase is 520 ℃, and the melting point of the first matrix phase is 475 ℃.
And re-heating the first alloy to 500 ℃ to melt the first matrix phase, wherein the Au-rich Au-Cu-Gd primary crystal phase is not melted to obtain a semi-solid alloy melt. The semi-solid alloy melt is spun by a copper roller at a speed of 10 DEG C6Cooling the solidification rate of K/s to room temperature to obtain a second alloy with the embedded primary crystal phase and the amorphous second matrix phase, wherein the second alloy is a thin strip with the thickness of 20 mu m. As shown in FIG. 1, the thickness of the primary crystal phase is about 450nm, the primary crystal phase is a regular hexagonal plate shape, and the circumscribed circle diameter of the regular hexagon is about 3 μm.
0.1 g of the second alloy obtained above was reacted with 30mL of a 3mol/L hydrochloric acid aqueous solution for 2 hours. In the reaction process, the second matrix phase is basically dissolved in an acid solution, and the separated Au-Cu-Gd primary crystal phase rich in Au further removes elements Cu and Gd. After separation and cleaning, the regular hexagonal sheet-shaped nano-porous Au material shown in fig. 2 and 3 is obtained, the thickness is about 450nm, the diameter of the circumscribed circle of the regular hexagon is about 3 μm, the average size of the nano-porous ligament is 40nm, and the energy spectrum is shown in fig. 4.
Example 2
Selected component is Mg61Cu20Au5Pt2Pd1Gd11The precursor alloy is prepared into alloy according to the element composition, the alloy is fully melted by induction, and then the alloy melt is solidified to room temperature at the speed of 10K/s to obtain the precursor alloy with the component of Mg61Cu20Au5Pt2Pd1Gd11The first alloy of (1). In the solidification process, an Au-Pt-Pd-rich primary crystal phase with the element composition of (Au-Pt-Pd) -Cu-Gd is firstly precipitated, and a residual melt with amorphous forming capability is solidified into a first matrix phase, wherein the melting point of the primary crystal phase is 525 ℃ and the melting point of the first matrix phase is 480 ℃.
The first alloy was reheated to 510 ℃ to melt the first matrix phase without melting the Au-Pt-Pd rich primary crystalline phase of elemental composition (Au-Pt-Pd) -Cu-Gd to obtain a semi-solid alloy melt. The semisolid alloy melt is subjected to a copper roller strip throwing technology-105And cooling the solidification rate of K/s to room temperature to obtain a second alloy with the embedded primary crystal phase and the amorphous second matrix phase, wherein the second alloy is a thin strip with the thickness of 40 mu m. The thickness of the primary crystal phase is about 500nm, the primary crystal phase is in the shape of a regular hexagonal plate, and the diameter of a circumscribed circle of the regular hexagon is about 4 mu m.
0.1 g of the second alloy obtained above was reacted with 50mL of a 1mol/L nitric acid aqueous solution for 1 hour. In the reaction process, the second matrix phase is basically dissolved in an acid solution, and the separated (Au-Pt-Pd) -Cu-Gd primary crystal phase further removes elements Cu and Gd. After separation and cleaning, the regular hexagonal sheet-shaped nano-porous Au-Pt-Pd material is obtained, the thickness is about 500nm, the diameter of a circumscribed circle of the regular hexagon is about 4 mu m, and the average size of a nano-porous frenulum is 50 nm.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method of preparing a nanoporous metal powder, comprising:
according to the formula MgaCubMcREdWeighing raw materials, wherein M is selected from at least one of Au, Pt, Pd, Ru, Rh and Ir, RE is at least one of rare earth elements, a, b, c and d respectively represent the atomic percentage content of each element, a is more than or equal to 55% and less than or equal to 70%, b is more than or equal to 15% and less than or equal to 25%, c is more than or equal to 2% and less than or equal to 10%, and a + b + c + d is 100%, melting the raw materials, and then cooling to room temperature at a first solidification rate to obtain a first alloy; the solidification structure of the first alloy comprises a primary crystal phase rich in M and at least one of Cu and RE, the primary crystal phase comprises M and at least one of Cu and RE, the primary crystal phase is in a shape of a sheet hexagon, and the melting point of the primary crystal phase is TmThe melting point of the first matrix phase is Tn，Tn<Tm；
Heating the first alloy to a temperature T, and then cooling to room temperature at a second solidification rate, the second solidification rate being greater than the first solidification rate, to obtain a second alloy, wherein T isn<T<TmSaidThe second alloy comprises an amorphous second matrix phase and the primary crystal phase distributed in the second matrix phase;
and providing an acid solution, mixing the second alloy with the acid solution, reacting the second matrix phase with the acid solution to obtain ions which enter the solution, separating the primary crystal phase out and reacting with the acid solution to obtain the nano-porous metal powder with the component M, wherein the nano-porous metal powder is sheet hexagonal particles and is in a nano-porous structure.
2. The method of claim 1, wherein the first solidification rate is 0.1K/s to 500K/s and the second solidification rate is 10K/s3K/s～107K/s。
3. The method of claim 1, wherein T isnAt 460 to 495 ℃, said TmIs 510 ℃ to 555 ℃.
4. The method of claim 1, wherein the thickness of the primary crystalline phase is 50nm to 1000 nm.
5. The method of claim 4, wherein the primary phase is in the shape of a regular hexagon in the form of a flake.
6. The method of claim 5, wherein the diameter of the circumscribed circle of the regular hexagon is 1 μm to 10 μm.
7. The method of claim 1, wherein the acid in the acid solution is at least one of hydrochloric acid, nitric acid, and sulfuric acid, and the molar concentration of the acid in the acid solution is 1mol/L to 10 mol/L.
8. The method for preparing nanoporous metal powder according to claim 1, wherein the temperature of the second alloy mixed with the acid solution is 0 ℃ to 100 ℃ and the reaction time is 10min to 3 h.
9. The method of claim 1, wherein the size of the porous ligaments in the nanoporous structure is between 20nm and 100 nm.
10. A nanoporous metal powder prepared by the method of any one of claims 1 to 9, wherein the nanoporous metal powder has a composition M selected from at least one of Au, Pt, Pd, Ru, Rh and Ir, and is in the form of sheet-like hexagonal particles having a nanoporous structure.
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| CN113649565A (en) * | 2020-09-30 | 2021-11-16 | 赵远云 | Alloy powder and preparation method and application thereof |
| CN113493876A (en) * | 2021-07-07 | 2021-10-12 | 重庆大学 | Method for modifying surface of magnesium alloy through iron-based amorphous modification |
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