CN114134362A - Preparation method of large-size high-strength three-stage composite porous magnesium-silver alloy - Google Patents

Preparation method of large-size high-strength three-stage composite porous magnesium-silver alloy Download PDF

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CN114134362A
CN114134362A CN202111371794.9A CN202111371794A CN114134362A CN 114134362 A CN114134362 A CN 114134362A CN 202111371794 A CN202111371794 A CN 202111371794A CN 114134362 A CN114134362 A CN 114134362A
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alloy
silver alloy
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李再久
李飞
杨秀苹
金青林
刘明昭
赵国荣
夏臣平
夏灿
夏丰领
刘恩典
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045—Directionally solidified castings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • C22C1/083—Foaming process in molten metal other than by powder metallurgy
    • C22C1/086—Gas foaming process
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver

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Abstract

The invention discloses a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy, which is characterized by comprising the following steps of: putting Mg and Ag into a crucible arranged on a water-cooled copper base, and vacuumizing; slowly preheating, increasing heating speed and introducing H2Heating to a specified temperature; after the alloy is melted, preserving heat for a certain time; the heating power supply is turned off, and the melt is meltedPouring the mixture into a graphite casting mould with a water-cooled copper bottom, cooling to room temperature, and carrying out pressure relief sampling; removing oil stain with alcohol or acetone, and polishing with sand paper; acid-eluting the alloy, cleaning with alcohol, naturally drying, and storing. The method is simple, efficient, low in cost and capable of being implemented on a large scale, the prepared nano porous metal material is uniform in thickness and pore distribution, can realize adjustability of structural parameters of the porous membrane, has the characteristics of high specific surface area, high electric conductivity and the like, is suitable for various substrates, and can be effectively applied to the fields of catalysis, electrochemistry, sensors, wave-absorbing devices, photoelectricity and the like.

Description

Preparation method of large-size high-strength three-stage composite porous magnesium-silver alloy
Technical Field
The invention belongs to the technical field of porous metal material preparation, and particularly relates to a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy.
Background
The nano porous material is a new material developed in recent decades, and has the structural characteristic that three-dimensional bicontinuous and mutually communicated nano-scale ligament/channel structures are dispersed and distributed in the material. The nano porous metal has the characteristics of high specific surface area, low density, high permeability, flexible and adjustable structure and the like, so that the nano porous metal has a huge application prospect in the fields of catalysis, sensing, optics and the like.
The methods mainly adopted by the current patents and documents related to the preparation of the nano porous material are a template method and an alloy removing method. Wherein: the 'template method' mainly takes porous alumina, liquid crystal phase or nano particles as a template, deposits a target metal material on the prefabricated porous template, and removes the template after deposition to obtain the porous metal material with the structure and the appearance similar to the template; the method has the advantages that the porous structure can be accurately controlled, and the defects that the size and the distribution arrangement mode of pores are determined by the template, the adjustment of the porous structure can only be controlled by the design of the template structure, the manufacturing cost is high, and the method is not suitable for batch production. The 'dealloying method' is that by using the electrode potential difference between the alloy components, one or more components with more active electrochemical properties in the alloy are selectively corroded through chemical or electrochemical corrosion, while inert components with relatively stable electrochemical properties can be diffused and aggregated, so that a bicontinuous nano porous structure is formed; the process has the advantages that the operation is simple, the pore structure can be regulated and controlled by the processes of corrosive agent selection, corrosion parameter control, subsequent heat treatment and the like, and the defect that the sample is required to be completely dealloyed, the sample has quite thin thickness (less than 100 micrometers), so that the nano porous material prepared by the dealloying method is extremely small in size and extremely high in brittleness, the application range and the prospect of the nano porous metal are limited undoubtedly, and the process is also a bottleneck and technical difficulty of the research of the nano porous material at present.
Therefore, based on the requirements of the field of macromolecular catalysis for the size of multistage pores, a new method for preparing a nano porous material with large size, high strength and efficient preparation process is urgently needed to prepare a three-stage composite porous material which is composed of a ligament/channel structure, has the characteristics of uniform pore distribution, adjustability of porous structure parameters, high specific surface area, high electric conductivity and the like, can be effectively applied to the fields of catalysis, electrochemistry, sensors, wave-absorbing devices, photoelectricity and the like and has wide application prospect.
Therefore, in order to solve the above problems, a method for preparing a large-sized high-strength three-stage composite porous magnesium-silver alloy is proposed herein.
Disclosure of Invention
In order to solve the technical problems, the invention designs a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy, which uses Mg-Ag alloy with micropores obtained by a directional solidification process as a precursor material, prepares a large-size micro-nano composite porous metal material by dealloying, and can obtain the multi-level porous metal material by adjusting the components of the precursor material.
In order to achieve the technical effects, the invention is realized by the following technical scheme: a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy is characterized by comprising the following steps:
s1: putting Mg and Ag into a crucible according to a certain atomic ratio, placing the crucible on a water-cooled copper base, and vacuumizing;
s2: when the air pressure is stable, a smelting power supply is turned on to smelt metal, the alloy is slowly preheated to be uniformly heated, the oxidation burning loss rate of the metal is reduced after the alloy reaches a certain temperature, the heating speed is increased, and H is introduced2Heating to a specified temperature;
s3: after the complete alloy is melted, preserving heat for a certain time at a set superheat degree;
s4: after the heat preservation time is reached, closing a heating power supply, pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification to obtain a GASAR porous magnesium silver alloy, and when the sample is cooled to room temperature, decompressing and sampling;
s5: sampling, namely sampling on the cast ingot, removing oil stains by using alcohol or acetone, and polishing by using abrasive paper;
s6: and (3) performing dealloying treatment on the sample in an acid solution to obtain the novel three-stage composite porous magnesium-silver alloy, cleaning the sample with alcohol after the corrosion is finished, naturally drying the sample, and storing the sample in vacuum.
Further, the atomic ratio of Mg to Ag alloy in S1 is Mg50Ag50-Mg99Ag1Pressure of 10-2Pa。
Further, in said S2, H2The purity of (2) is 99.99%, and the designated temperature is 950 ℃; and the heat preservation time in S3 is 30-40 min.
Further, in the S6, the acidic solution includes, but is not limited to, a 1% -20% HCl solution, a H2SO4 solution, a H3PO4 solution, and a C2H2O4 solution.
The invention has the beneficial effects that:
the invention designs a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy, which comprises the steps of obtaining a micron-pore Mg-Ag alloy as a precursor material by a directional solidification process, preparing a large-size micro-nano composite porous metal material by dealloying, obtaining a multi-level pore metal material by adjusting the components of the precursor material, and obtaining a three-stage porous material, namely micron, submicron and nano-level composite porous materials by adjusting the proportion of alloy elements; the invention provides a simple, high-efficiency, low-cost and large-scale implementation method for preparing a porous nano metal film, so that the prepared porous nano metal film consists of metal nano fibers, has uniform thickness and pore distribution, can realize the adjustability of structural parameters of a porous film, has the characteristics of high specific surface area, high electric conductivity and the like, is suitable for various substrates, can be effectively applied to the fields of catalysis, electrochemistry, sensors, wave-absorbing devices, photoelectricity and the like, and has wide application prospect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is the micropore morphology of the GASAR Mg-Ag alloy prepared in example 4;
FIG. 2 shows the sub-micron pore morphology obtained after dealloying the GASAR Mg-Ag alloy prepared in example 4;
FIG. 3 shows the nanopore morphology obtained after dealloying the GASAR Mg-Ag alloy prepared in example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1 to 3, a method for preparing a large-size high-strength three-stage composite porous magnesium-silver alloy is characterized in that:
s1: putting Mg and Ag into a crucible according to a certain atomic ratio, placing the crucible on a water-cooled copper base, and vacuumizing;
s2: when the air pressure is stable, a smelting power supply is turned on to smelt metal, the alloy is slowly preheated to be uniformly heated, the oxidation burning loss rate of the metal is reduced after the alloy reaches a certain temperature, the heating speed is increased, and H is introduced2Heating to a specified temperature;
s3: after the complete alloy is melted, preserving heat for a certain time at a set superheat degree;
s4: after the heat preservation time is reached, closing a heating power supply, pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification to obtain a GASAR porous magnesium silver alloy, and when the sample is cooled to room temperature, decompressing and sampling;
s5: sampling, namely sampling on the cast ingot, removing oil stains by using alcohol or acetone, and polishing by using abrasive paper;
s6: and (3) performing dealloying treatment on the sample in an acid solution to obtain the novel three-stage composite porous magnesium-silver alloy, cleaning the sample with alcohol after the corrosion is finished, naturally drying the sample, and storing the sample in vacuum.
The atomic ratio of Mg to Ag alloy in S1 is Mg50Ag50-Mg99Ag1。
In the S2, H2The purity of (2) is 99.99%, and the designated temperature is 950 ℃; and the heat preservation time in S3 is 30-40 min.
In the S6, the acidic solution includes but is not limited to a 1% -20% HCl solution, a H2SO4 solution, a H3PO4 solution, and a C2H2O4 solution.
Example 2
The method comprises the following specific steps:
(1) polishing the surface of Mg-Ag alloy until no dirt exists, putting the Mg-Ag alloy into a crucible in a furnace, covering a furnace cover tightly, and vacuumizing to 10 DEG- 2Pa。
(2) After the gas pressure in the furnace is stable, metal is smelted, the alloy is slowly preheated to be uniformly heated, after a certain temperature is reached, the heating rate is increased for reducing the metal oxidation burning loss, H2 is introduced, and the alloy is heated to the specified temperature.
(3) And after the alloy is completely melted, preserving the heat for 30min at the set superheat degree.
(4) And after the heat preservation time is reached, closing the heating power supply, and pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification. And (5) when the sample is cooled to room temperature, decompressing and sampling.
(5) Sampling, taking the sample from the ingot
Figure BDA0003362527870000062
Removing oil stain with alcohol or acetone, and polishing with sand paper.
(6) And (3) performing dealloying treatment on the sample in an acid solution, cleaning the sample by using alcohol and pure water after corrosion is finished, and drying the sample in a vacuum drying oven.
Example 3
According to atomic percent as Mg95Ag5Preparing precursor material according to the proportion, polishing the alloy, placing the alloy into a crucible in a furnace, covering a furnace cover tightly, and vacuumizing to 10 DEG-2Pa. After the gas pressure in the furnace is stable, the metal is smelted, firstly, the alloy is slowly preheated to be uniformly heated, after a certain temperature is reached, the heating rate is increased for reducing the oxidation burning loss of the metal, and H is introduced2And heating to a specified temperature, and preserving the heat for 30min at a set superheat degree after the alloy is completely melted. And after the heat preservation time is reached, closing the heating power supply, and pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification. And (5) when the sample is cooled to room temperature, decompressing and sampling. Taking out from cast ingot
Figure BDA0003362527870000061
The sample is degreased with alcohol or acetone and then sanded with sand paper. Performing dealloying treatment on the sample in a hydrochloric acid solution with the mass fraction of 1%, cleaning the sample with alcohol and pure water after the corrosion is finished, and performing vacuum drying in a vacuum drying ovenThe sample was dried.
Example 4
According to atomic percent as Mg80Ag20Preparing precursor material according to the proportion, polishing the alloy, placing the alloy into a crucible in a furnace, covering a furnace cover tightly, and vacuumizing to 10 DEG-2Pa. After the gas pressure in the furnace is stable, the metal is smelted, firstly, the alloy is slowly preheated to be uniformly heated, after a certain temperature is reached, the heating rate is increased for reducing the oxidation burning loss of the metal, and H is introduced2And heating to a specified temperature, and preserving the heat for 30min at a set superheat degree after the alloy is completely melted. And after the heat preservation time is reached, closing the heating power supply, and pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification. And (5) when the sample is cooled to room temperature, decompressing and sampling. Taking out from cast ingot
Figure BDA0003362527870000072
The sample is degreased with alcohol or acetone and then sanded with sand paper. And (3) performing dealloying treatment on the sample in a hydrochloric acid solution with the mass fraction of 1%, cleaning the sample by using alcohol and pure water after the corrosion is finished, and drying the sample in a vacuum drying oven.
Example 5
According to atomic percent as Mg65Ag35Preparing precursor material according to the proportion, polishing the alloy, placing the alloy into a crucible in a furnace, covering a furnace cover tightly, and vacuumizing to 10 DEG-2Pa. After the gas pressure in the furnace is stable, the metal is smelted, firstly, the alloy is slowly preheated to be uniformly heated, after a certain temperature is reached, the heating rate is increased for reducing the oxidation burning loss of the metal, and H is introduced2And heating to a specified temperature, and preserving the heat for 30min at a set superheat degree after the alloy is completely melted. And after the heat preservation time is reached, closing the heating power supply, and pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification. And (5) when the sample is cooled to room temperature, decompressing and sampling. Taking out from cast ingot
Figure BDA0003362527870000071
The sample is degreased with alcohol or acetone and then sanded with sand paper. The sample is subjected to dehydration in a hydrochloric acid solution with the mass fraction of 1%And (4) gold treatment, cleaning with alcohol and pure water after corrosion is finished, and drying the sample in a vacuum drying oven.
Example 6
According to atomic percent as Mg50Ag50Preparing precursor material according to the proportion, polishing the alloy, placing the alloy into a crucible in a furnace, covering a furnace cover tightly, and vacuumizing to 10 DEG-2Pa. After the gas pressure in the furnace is stable, the metal is smelted, firstly, the alloy is slowly preheated to be uniformly heated, after a certain temperature is reached, the heating rate is increased for reducing the oxidation burning loss of the metal, and H is introduced2And heating to a specified temperature, and preserving the heat for 30min at a set superheat degree after the alloy is completely melted. And after the heat preservation time is reached, closing the heating power supply, and pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification. And (5) when the sample is cooled to room temperature, decompressing and sampling. Taking out from cast ingot
Figure BDA0003362527870000081
The sample is degreased with alcohol or acetone and then sanded with sand paper. And (3) performing dealloying treatment on the sample in a hydrochloric acid solution with the mass fraction of 5%, cleaning the sample by using alcohol and pure water after the corrosion is finished, and drying the sample in a vacuum drying oven.
Example 7
The large-size high-strength three-level composite porous magnesium-silver alloy prepared by the method has the porosity of 5-90 percent, the micron aperture of 50-5000 microns and the submicron aperture of 200-800 nanometers; the size can reach: length (1-1000mm), width (1-1000mm), height (1-50mm), its surface area can be up to 80 square meters/gram-150 square meters/gram.
Example 8
The invention designs a preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy, which comprises the steps of obtaining a micron-pore Mg-Ag alloy as a precursor material by a directional solidification process, preparing a large-size micro-nano composite porous metal material by dealloying, obtaining a multi-level pore metal material by adjusting the components of the precursor material, and obtaining a three-stage porous material, namely micron, submicron and nano-level composite porous materials by adjusting the proportion of alloy elements; the invention provides a simple, high-efficiency, low-cost and large-scale implementation method for preparing a porous nano metal film, so that the prepared porous nano metal film consists of metal nano fibers, has uniform thickness and pore distribution, can realize the adjustability of structural parameters of a porous film, has the characteristics of high specific surface area, high electric conductivity and the like, is suitable for various substrates, can be effectively applied to the fields of catalysis, electrochemistry, sensors, wave-absorbing devices, photoelectricity and the like, and has wide application prospect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (5)

1. A preparation method of a large-size high-strength three-stage composite porous magnesium-silver alloy is characterized by comprising the following steps:
s1: putting Mg and Ag into a crucible according to a certain atomic ratio, placing the crucible on a water-cooled copper base, and vacuumizing;
s2: when the air pressure is stable, a smelting power supply is turned on to smelt metal, the alloy is slowly preheated to be uniformly heated, and when the air pressure reaches the range of the melting power supply, the alloy is heatedAfter a certain temperature, in order to reduce the metal oxidation burning loss rate, increase the heating speed and introduce H2Heating to a specified temperature;
s3: after the complete alloy is melted, preserving heat for a certain time at a set superheat degree;
s4: after the heat preservation time is reached, closing a heating power supply, pouring the melt into a graphite casting mold with a water-cooled copper bottom for directional solidification to obtain a GASAR porous magnesium silver alloy, and when the sample is cooled to room temperature, decompressing and sampling;
s5: sampling, namely sampling on the cast ingot, removing oil stains by using alcohol or acetone, and polishing by using abrasive paper;
s6: and (3) performing dealloying treatment on the sample in an acid solution to obtain the novel three-stage composite porous magnesium-silver alloy, cleaning the sample with alcohol after the corrosion is finished, naturally drying the sample, and storing the sample in vacuum.
2. The preparation method of the large-size high-strength three-stage composite porous magnesium-silver alloy according to claim 1, wherein the preparation method comprises the following steps: the atomic ratio of Mg to Ag alloy in S1 is Mg50Ag50-Mg99Ag1Pressure of 10-2Pa。
3. The preparation method of the large-size high-strength three-stage composite porous magnesium-silver alloy according to claim 1, wherein the preparation method comprises the following steps: in the S2, H2The purity of (2) is 99.99%, and the designated temperature is 950 ℃; and the heat preservation time in S3 is 30-40 min.
4. The preparation method of the large-size high-strength three-stage composite porous magnesium-silver alloy according to claim 1, wherein the preparation method comprises the following steps: in the S6, the acidic solution includes but is not limited to a 1% -20% HCl solution, a H2SO4 solution, a H3PO4 solution, and a C2H2O4 solution.
5. The preparation method of the large-size high-strength three-stage composite porous magnesium-silver alloy according to any one of claims 1 to 4, which discloses the application of the preparation method of the large-size high-strength three-stage composite porous magnesium-silver alloy in the technical field of porous metal material preparation.
CN202111371794.9A 2021-11-18 2021-11-18 Preparation method of large-size high-strength three-stage composite porous magnesium-silver alloy Pending CN114134362A (en)

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CN114589314A (en) * 2022-03-07 2022-06-07 中南大学 Preparation method of porous metal material with secondary porous structure

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