CN109355516B - Porous nickel alloy and preparation method thereof - Google Patents
Porous nickel alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22C1/023—Alloys based on nickel
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
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- C22C30/06—Alloys containing less than 50% by weight of each constituent containing zinc
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Abstract
A porous nickel alloy and a preparation method thereof are disclosed, wherein the porous nickel alloy comprises the following chemical components in percentage by mass: cu: 1-30%, Zn is less than or equal to 5%, Mn is less than or equal to 2%, Sn: 2-20%, Ga: 0.1-15%, less than or equal to 5% of Mg, less than or equal to 5% of Al, and the balance of Ni and inevitable impurities. The preparation method comprises the following steps: (1) melting the alloy raw materials, casting and cooling to obtain a nickel alloy precursor cast ingot; (2) cutting and polishing the nickel alloy precursor cast ingot to obtain a nickel alloy precursor sample; (3) and carrying out vacuum heat treatment on the nickel alloy precursor sample at the temperature of 450-700 ℃, and carrying out heat preservation or temperature change treatment in a continuous vacuum environment to obtain the porous nickel alloy. The process method is simple and suitable for large-scale production, and the obtained product has adjustable porosity and can be applied to the fields of fuel cell frames, separation, filtration, catalysis, noise reduction, shock absorption, shielding, heat exchange and the like.
Description
Technical Field
The invention belongs to the field of metal materials, and particularly provides a porous nickel alloy and a preparation method thereof.
Background
In recent years, the development and application of metal porous materials are receiving increasing attention, and metal porous materials (foam metal) are novel engineering materials which are composed of rigid frameworks and internal pores, have excellent physical properties and good mechanical properties, and are rapidly developed in the later 80 s of the 20 th century. The material has excellent physical properties (such as small density, large rigidity, large specific surface area, good energy absorption and vibration reduction performance, good noise reduction effect, high electromagnetic shielding performance and the like), so that the application field of the material is expanded to the fields of aviation, electronics, medical materials, biochemistry and the like. The metal porous material with the through holes also has the advantages of strong heat exchange and heat dissipation capacity, good permeability, high thermal conductivity and the like, and has wide application prospects in the fields of aviation, aerospace, chemical engineering, building materials, metallurgy, atomic energy, petrifaction, machinery, medicine, environmental protection and the like. Porous nickel or foamed nickel is widely applied to battery electrode materials, filter carriers, chemical catalyst carriers, electromagnetic shielding materials, noble metal replacement and recovery and other fields at present.
Since the beginning of the 20 th century, mankind has made porous metal materials by powder metallurgy, the history of porous metal production has been over a hundred years, and the traditional production methods mainly include: powder sintered type, fiber sintered type, composite type, deposition type, corrosion type, and the like. The template method is an important method for synthesizing a porous material, which has been developed in recent years, and is a method of filling a raw material in pores of a template material using a colloidal crystal as a template, and removing the template material by a physical or chemical method to obtain an inverse replica of the template material, i.e., a porous material. The selection of the template is the core step of the method, determining the structure and properties of the porous material. The process of either the template method or the powder sintering method is relatively complicated.
A porous matrix foamed plastic is adopted, a conductive layer is prepared by chemical nickel plating, vacuum nickel plating and other methods, thick nickel is electroplated in sulfate nickel plating electrolyte after nickel preplating, and then the three-dimensional reticular foamed nickel material with excellent performance can be obtained through firing, reducing and annealing processes. The pore diameter of the porous nickel alloy prepared by the method is usually limited by the pore diameter of the matrix foam, and the pore diameter is usually larger.
The dealloying method is a method for preparing nano porous material, and can also be used for preparing porous nickel alloy, but the method belongs to dealloying corrosion, and is generally carried out on the surface layer of metal material when being used for preparing porous metal material, so that the bulk material is difficult to prepare. The invention provides a method for preparing porous nickel alloy with micron-sized and below-micron-sized dimensions on a large scale, which is used for meeting the application of porous nickel in the fields of energy, aviation, aerospace, chemical engineering, building materials, metallurgy, atomic energy, petrifaction, machinery, medicine, environmental protection and the like.
Disclosure of Invention
The invention aims to provide a porous nickel alloy and a preparation method thereof, and the porous nickel alloy with a three-dimensional through hole structure is prepared by a vacuum heat treatment process.
The invention particularly provides a porous nickel alloy which is characterized by comprising the following chemical components in percentage by mass: cu: 1-30%, Zn is less than or equal to 5%, Mn is less than or equal to 2%, Sn: 2-20%, Ga: 0.1-15%, less than or equal to 5% of Mg, less than or equal to 5% of Al, and the balance of Ni and inevitable impurities.
The porous nickel alloy has a pore diameter of 0.1-50 μm and a porosity of 30-70%.
The porous nickel alloy can be applied to the fields of fuel cell frames, separation, filtration, catalysis, noise reduction, shock absorption, shielding and heat exchange.
The invention also provides a preparation method of the porous nickel alloy, which is characterized by comprising the following steps:
(1) preparing a nickel alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Cu: 1-30%, Zn: 30-60%, Mn: 2-12%, Sn: 2-20%, Ga: 0.1-15%, Mg: 1-6%, Al is less than or equal to 5%, Ni: the balance of Ni and inevitable impurities, melting the raw materials, casting, and cooling to obtain a nickel alloy precursor ingot;
(2) processing a nickel alloy precursor ingot: cutting and polishing the nickel alloy precursor cast ingot to obtain a nickel alloy precursor sample;
(3) preparing a porous nickel alloy: and carrying out vacuum heat treatment on the nickel alloy precursor sample at the temperature of 450-700 ℃, and carrying out heat preservation or temperature change treatment in a continuous vacuum environment, wherein the vacuum degree is less than or equal to 10pa, and the treatment time is more than or equal to 1h, so as to obtain the porous nickel alloy.
In the step (1), one or more of mercury, indium, bismuth, cadmium, antimony or lead is added into the nickel alloy precursor, and the adding amount is less than or equal to 1 (wt)%, calculated by the mass of the nickel alloy precursor.
In the step (1), the melting step is to add the nickel alloy precursor raw material into a crucible of a resistance furnace or an induction furnace for heating and melting.
In the step (2), the nickel alloy precursor ingot is cut, and the polishing step is to cut the nickel alloy precursor ingot by using a linear cutting machine, and then polish and polish the ingot by using water sand paper to obtain a nickel alloy precursor sample; or forging the nickel alloy precursor ingot into a plate or a bar, then cutting the plate or the bar into samples by adopting the method, and polishing to obtain the nickel alloy precursor sample.
In the step (3), the vacuum heat treatment is performed in a vacuum heat treatment furnace.
In the step (3), the temperature change treatment is carried out at 450-700 ℃ and the heating rate is 5-100 ℃/h.
In the step (3), the nickel alloy precursor sample is pretreated before vacuum heat treatment, and the pretreatment method is one or more of high-temperature quenching, plastic deformation or high-energy particle irradiation.
Firstly, the preparation method of the porous nickel alloy mainly utilizes unbalanced diffusion (the kirkendall effect), a large amount of alloy elements with high diffusion coefficients are added into a nickel alloy precursor, more vacancies can be formed in a matrix at the temperature of 400-800 ℃ because the diffusion rate of the alloy elements is far greater than that of the matrix nickel elements, and when the vacancies are accumulated to a certain degree, a large amount of vacancies are combined into a plurality of holes, so that the porous nickel alloy is finally formed.
In order to accelerate the formation of the porous nickel alloy, elements of manganese, zinc and magnesium with high vapor pressure are added into the alloy, and the manganese, the zinc and the magnesium can be completely or partially removed through sublimation at the temperature of 400-800 ℃, so that the concentration gradient of diffusion vacancies is increased, and the formation of the vacancies is accelerated and the formation of the porous nickel alloy is promoted. Manganese, zinc and magnesium in the alloy may not be the final alloying elements, but may be one of the alloying elements depending on the end use, while copper, tin, gallium, aluminum and lithium are the final alloying elements of the porous nickel alloy.
Secondly, the diffusion of the alloy elements is influenced by temperature and time, different alloy elements and matrix nickel elements have the optimal temperature and have the maximum diffusion speed difference, the lower temperature causes the diffusion rate to be too slow to form a large number of vacancy pore-forming holes, and the higher temperature easily causes the formed holes to be closed at high temperature. The method is characterized by carrying out heat preservation or temperature change treatment in a continuous vacuum environment at 400-800 ℃, wherein the temperature change treatment is that the temperature is slowly increased from 450 ℃ to 700 ℃; the heat preservation treatment time of different temperature sections is determined by the type and the content of the alloy, the total treatment time is increased according to the increase of the size of the sample, and the treatment time is more than or equal to 1 hour.
Meanwhile, the reduction of the environmental pressure can promote the diffusion rate, and in order to increase the diffusion rate, the treatment process of the porous nickel alloy is a continuous vacuum environment.
The shape of the porous nickel alloy of the present invention is not limited to a bulk, and may be a foil, a powder, or the like.
The invention has the advantages that:
(1) the alloy components can form solid solution with the nickel base, the preparation process of the alloy is simple, the porous nickel alloy adopts a vacuum heat treatment process, large-scale production can be carried out, and the preparation method not only can be used for preparing large-size blocks, but also is particularly suitable for preparing ultrathin porous nickel foils and porous nickel powder or nickel balls;
(2) the porous pure alloy prepared by the process has a through hole structure, and the porosity of the porous pure alloy is adjustable according to the proportion of alloy components;
(3) the porous nickel alloy prepared by the process can be applied to the fields of fuel cell frames, separation, filtration, catalysis, noise reduction, shock absorption, shielding, heat exchange and the like.
Drawings
Figure 1 picture of three-dimensional porous nickel alloy obtained in example 1.
Detailed Description
The following examples further illustrate the invention but are not intended to limit the invention thereto.
All percentages in this example are expressed as mass percentages unless otherwise specified.
Example 1
(1) Preparation of Ni34Mn5Zn50Sn6Cu2Mg2 AlGaNi alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Zn: 50%, Mn: 5%, Sn: 6%, Cu: 2%, Mg: 2%, Ni: 34 percent, and the balance of 1 percent is aluminum and gallium elements, the raw materials are added into a crucible of a resistance furnace, after the alloy is completely melted uniformly, casting is carried out, and a nickel alloy precursor ingot is obtained after cooling;
(2) cutting an Ni34Mn5Zn50Sn6Cu2Mg2 AlGaNi alloy precursor ingot to obtain a 20 × 20 × 1mm small piece, suspending the small piece in a quartz furnace tube of a vacuum heat treatment furnace, keeping the temperature at 500 ℃ for 5 hours under high vacuum, then keeping the temperature at 700 ℃ for 2 hours, keeping the vacuum degree within 10Pa to obtain the three-dimensional porous nickel alloy, wherein the aperture is 2-5 mu m, the porosity is 40%, and the picture of the porous nickel alloy is shown in figure 1.
Example 2
(1) Preparing a Ni40Zn40Cu8Sn7Mn3GaMgAl nickel alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Cu: 8%, Zn: 40%, Sn: 7%, Mn: 3%, Ni: 40 percent, and the balance of 2 percent of gallium, magnesium and aluminum elements, adding the raw materials into a crucible of an induction furnace, casting after the alloy is completely and uniformly melted, and cooling to obtain a nickel alloy precursor ingot;
(2) and cutting the Ni40Zn40Cu8Sn7Mn3GaMgAl nickel alloy precursor ingot to obtain 10 × 10 × 0.5.5 mm small pieces, hanging the small pieces in a small vacuum heat treatment furnace in a laboratory, keeping the temperature at 500 ℃ for 4 hours under high vacuum, and keeping the vacuum degree within 10Pa to obtain the three-dimensional porous nickel alloy, wherein the aperture is 2-10 mu m, and the porosity is 50%.
Example 3
(1) Preparing a Ni40Zn40Ga10Mn5Mg3AlSnCu nickel alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Zn: 40%, Ga: 10%, Mn: 5%, Mg: 3%, Ni: 40 percent, and the balance of 2 percent of aluminum, tin and copper elements, adding the raw materials into a crucible of a resistance furnace, casting after the alloy is completely and uniformly melted, and cooling to obtain a nickel alloy precursor ingot;
(2) the Ni40Zn40Ga10Mn5Mg3AlSnCu nickel alloy precursor is cast into a sheet with the thickness of 20 × 20 × 0.5.5 mm through wire cutting, the sheet is polished to be 0.3mm thick by abrasive paper, the sheet is hung in a small vacuum heat treatment furnace in a laboratory, the temperature is kept at 500 ℃ for 2 hours, then the temperature is kept at 600 ℃ for 1 hour, the high vacuum is continuously carried out, the vacuum degree is kept within 10Pa, and the three-dimensional porous nickel alloy is obtained, wherein the aperture is 2-10 mu m, and the porosity is 50%.
Example 4
(1) Preparing a Ni30Zn40Cu10Sn8Mg5Mn5GaAl nickel alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Cu: 10%, Zn: 40%, Sn: 8%, Mg: 5%, Mn: 5%, Ni: 30 percent, and the balance of 2 percent is aluminum and gallium elements. And adding the raw materials into a crucible of a resistance furnace, casting after the alloy is completely and uniformly melted, and cooling to obtain the nickel alloy precursor ingot.
(2) The method comprises the following steps of carrying out wire cutting on a Ni30Zn40Cu10Sn8Mg5Mn5GaAl nickel alloy precursor cast ingot into sheets with the thickness of 10 × 15 × 1mm, polishing the sheets to the thickness of 0.8mm by using abrasive paper, hanging the sheets in a small vacuum heat treatment furnace in a laboratory, pretreating the sheets for 2 hours at 450 ℃, then gradually raising the temperature to 550 ℃, carrying out heat preservation for 6 hours at 550 ℃, keeping high vacuum continuously, and keeping the vacuum degree within 10Pa to obtain the three-dimensional porous nickel alloy, wherein the pore diameter is 1-20 mu m, and the porosity is 60%.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. The porous nickel alloy is characterized by comprising the following chemical components in percentage by mass: cu: 1-30%, Zn is less than or equal to 5%, Mn is less than or equal to 2%, Sn: 2-20%, Ga: 0.1-15%, less than or equal to 5% of Mg, less than or equal to 5% of Al, and the balance of Ni and inevitable impurities; the porous nickel alloy has a pore diameter of 0.1-50 μm and a porosity of 30-70%.
2. The method of claim 1, wherein the steps of:
(1) preparing a nickel alloy precursor: according to the chemical composition and mass percentage of the nickel alloy precursor, Cu: 1-30%, Zn: 30-60%, Mn: 2-12%, Sn: 2-20%, Ga: 0.1-15%, Mg: 1-6%, Al is less than or equal to 5%, Ni: the balance of Ni and inevitable impurities, melting the raw materials, casting, and cooling to obtain a nickel alloy precursor ingot;
(2) processing a nickel alloy precursor ingot: cutting and polishing the nickel alloy precursor cast ingot to obtain a nickel alloy precursor sample;
(3) preparing a porous nickel alloy: and carrying out vacuum heat treatment on the nickel alloy precursor sample at the temperature of 450-700 ℃, and carrying out heat preservation or temperature change treatment in a continuous vacuum environment, wherein the vacuum degree is less than or equal to 10Pa, and the treatment time is more than or equal to 1h, so as to obtain the porous nickel alloy.
3. The preparation method according to claim 2, wherein in the step (1), one or more of mercury, indium, bismuth, cadmium, antimony or lead is added to the nickel alloy precursor, and the addition amount is less than or equal to 1 (wt)%, calculated by the mass of the nickel alloy precursor.
4. The preparation method according to claim 2, wherein in the step (1), the melting step is to add the nickel alloy precursor raw material into a crucible of a resistance furnace or an induction furnace for heating and melting.
5. The preparation method according to claim 2, wherein in the step (2), the nickel alloy precursor ingot is cut, and the polishing step is to cut the nickel alloy precursor ingot by using a linear cutting machine, and then polish and polish the ingot by using water sand paper to obtain a nickel alloy precursor sample; or forging the nickel alloy precursor ingot into a plate or a bar, then cutting the plate or the bar into samples by adopting the method, and polishing to obtain the nickel alloy precursor sample.
6. The method according to claim 2, wherein in the step (3), the vacuum heat treatment is performed in a vacuum heat treatment furnace.
7. The preparation method according to claim 2, wherein in the step (3), the temperature-changing treatment is performed at a temperature-changing rate of 5-100 ℃/h within a range of 450-700 ℃.
8. The method according to claim 2, wherein in the step (3), the nickel alloy precursor sample is pretreated before vacuum heat treatment, and the pretreatment method is one or more of high temperature quenching, plastic deformation or high energy particle irradiation.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3841868A (en) * | 1972-12-22 | 1974-10-15 | Howmedica | Nickel alloys |
| JPS5567336A (en) * | 1978-11-16 | 1980-05-21 | Mitsubishi Heavy Ind Ltd | Preparation of catalyst |
| CN103627920A (en) * | 2013-11-11 | 2014-03-12 | 江苏大学 | Preparation method of porous nickel |
| CN105018770A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Method for preparing porous metal material and application thereof |
| CN105018771A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Preparation method of nickel foam or nickel foam substrate alloy |
| CN106801159A (en) * | 2015-11-26 | 2017-06-06 | 常德力元新材料有限责任公司 | A kind of preparation method of nickel foam or foam nickel-base alloy |
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- 2018-11-08 CN CN201811324454.9A patent/CN109355516B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3841868A (en) * | 1972-12-22 | 1974-10-15 | Howmedica | Nickel alloys |
| JPS5567336A (en) * | 1978-11-16 | 1980-05-21 | Mitsubishi Heavy Ind Ltd | Preparation of catalyst |
| CN103627920A (en) * | 2013-11-11 | 2014-03-12 | 江苏大学 | Preparation method of porous nickel |
| CN105018770A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Method for preparing porous metal material and application thereof |
| CN105018771A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Preparation method of nickel foam or nickel foam substrate alloy |
| CN106801159A (en) * | 2015-11-26 | 2017-06-06 | 常德力元新材料有限责任公司 | A kind of preparation method of nickel foam or foam nickel-base alloy |
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