CN114734043B - Preparation method of flaky metal powder - Google Patents
Preparation method of flaky metal powder Download PDFInfo
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- CN114734043B CN114734043B CN202210197448.1A CN202210197448A CN114734043B CN 114734043 B CN114734043 B CN 114734043B CN 202210197448 A CN202210197448 A CN 202210197448A CN 114734043 B CN114734043 B CN 114734043B
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
- C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a preparation method of high-density flaky metal powder, and belongs to the technical field of powder metallurgy. The invention adopts the process steps of raw material mixing, melting, gas atomization powder preparation, screening and the like to realize the preparation of the flaky metal powder. The invention adopts the technical ideas of low superheat degree, high catheter aperture and low pressure gas atomization, improves the viscosity of atomized melt, reduces the energy input of melt with unit mass, and changes the shape of gas atomized powder from spherical to lamellar. The obtained flaky metal powder has the advantages of large width-to-thickness dimension ratio, less impurities, large yield, low oxygen content and the like. The obtained sheet metal powder is in the shape of regular or irregular salix leaf with microcrystalline, nanocrystalline or amorphous structure. The method and the equipment have simple process, high efficiency and high powder quality, and are suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of metal powder preparation, in particular to a preparation method of flaky metal powder.
Background
The flaky metal powder is valued and has obtained a series of applications in the aspects of composite materials, wave absorbing materials, magnetic materials, pigments, conductive pastes and the like because of the characteristics and advantages of high specific surface area, high thickness-to-diameter ratio, directivity and the like. For example, flaky aluminum powder has silvery white metallic luster, and is one of the most widely used metallic pigments at present; flake copper and copper zinc alloy powders can be processed into commercial "copper gold powders"; flake silver powder and gold powder are used for preparing a conductive medium of conductive paste in the electronic industry; iron-based powder is widely used in the field of electromagnetic wave shielding and absorption.
At present, the preparation technology of the flaky metal powder mainly adopts a high-energy ball milling method and a chemical method. Chinese patent (CN 101829787 a) describes a method and apparatus for processing ultrafine flake powder, wherein a cylindrical ball milling tank is used, in which pier-type grid columns are arranged, and the cylindrical ball milling tank is filled with rigid grinding balls and ball milled for 8-16 hours to prepare flake metal powder. Chinese patent (CN 111069625 a) discloses a method for preparing flaky platinum nanoparticles, which adopts a chemical deposition method to heat, stir, reduce, separate and dry a platinum precursor, thereby obtaining flaky platinum nanoparticles. Both the high-energy ball milling method and the chemical method can realize the preparation of the flaky metal powder, but have respective disadvantages. For example, the high-energy ball milling method generally needs to prepare spherical powder in advance, then ball milling is carried out by a dry method or a wet method, then the powder preparation is realized by a step of drying and separating, the process operation is complicated, the process period is long, the processed material can be subjected to a work hardening phenomenon, the subsequent deformation difficulty phenomenon is caused, and the prepared flaky powder has the defects of irregular shape, serious oxidation, low purity and the like. Particularly for partially hard brittle metals and intermetallic compounds, flakes are difficult to prepare by high energy ball milling. The chemical method generally uses a metal salt reagent with higher purity, and the metal salt reagent is prepared by a reduction method, sintering or drying, so that the environmental pollution is easily caused, and the preparation cost is higher due to the complex manufacturing process.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a preparation method of the aerosolized flaky metal powder with short flow, low cost and batch.
The invention is realized by the following technical scheme.
A method for preparing sheet metal powder, the method comprising:
(1) Heating, stirring and overheat preserving the metal raw material under the condition that the vacuum degree is less than 100Pa to obtain molten metal liquid, wherein the overheat degree is 50-300 ℃, and the overheat preserving time is 1-30 min;
(2) Introducing atomizing gas into the molten metal liquid obtained in the step (1) for atomization to obtain flaky powder;
(3) And (3) completely cooling the flaky powder obtained in the step (2), and screening.
Further, the molten metal in the step (1) is composed of one or more elements of Fe, ni, W, al, cu, B, co.
Further, the step (1) adopts resistance heating or induction heating to heat the metal raw material.
Further, the molten metal is poured into the diversion crucible in the step (2) so that the molten metal continuously flows out along the liquid guide pipe on the diversion crucible.
Further, the diversion crucible is a crucible made of alumina or magnesia, and the diameter of the liquid guiding pipe is 3-8 mm.
Further, the atomizing gas in the step (2) is inert gas, and the gas pressure in the atomizing process is 2-6 MPa.
Further, the atomizing gas is nitrogen or argon.
The invention has the beneficial technical effects that the low-cost and short-flow preparation of the flaky metal powder is realized by adopting the gas atomization powder preparation process, and the industrialized batch production is expected to be realized. By adopting the technical ideas of low superheat degree, high catheter aperture and low-pressure gas atomization, the viscosity of the atomized melt is improved, the energy input of the melt with unit mass is reduced, and the shape of the gas atomized powder is changed from spherical to lamellar. The obtained flaky metal powder has the advantages of large width-to-thickness dimension ratio, less impurities, large yield, small stress, low oxygen content and the like. The obtained sheet metal powder is in the shape of regular or irregular salix leaf with microcrystalline, nanocrystalline or amorphous structure. The method and the equipment have simple process, high efficiency and high powder quality, and are suitable for industrial production.
Drawings
FIG. 1 is a photograph of a cross-sectional Scanning Electron Microscope (SEM) micrograph of an iron-based flaky powder prepared in example 1 of the present invention.
FIG. 2 is a photograph of a cross-sectional Scanning Electron Microscope (SEM) of an iron-nickel-based flaky powder prepared in example 2 of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention aims to develop a short-flow, low-cost and batched preparation method of the gas-atomized flaky metal powder, which aims at overcoming the defects of complex preparation flow, long period and high cost of the existing flaky metal powder.
The preparation process of the flaky metal powder material comprises the following steps:
(1) Loading the metal raw material into a crucible, heating the metal raw material by adopting resistance heating or induction heating under the vacuum degree of less than 100Pa, stirring and overheat preserving the heat to obtain molten metal, wherein the molten metal consists of one or more elements in Fe, ni, W, al, cu, B, co, the overheat degree is 50-300 ℃, and the overheat preserving time is 1-30 min;
(2) Closing the vacuum system, pouring molten metal into the diversion crucible, and enabling the molten metal to continuously flow out along a liquid guide pipe on the diversion crucible and enter an atomization bin; the diversion crucible is made of alumina or magnesia, and the diameter of the liquid guiding pipe is 3-8 mm;
(3) Opening an atomizing gas valve to introduce atomizing gas into the molten metal liquid for atomizing, adjusting the gas pressure, and forming sheet-shaped powder by metal liquid drops under the impact of high-pressure gas; wherein the atomizing gas is inert gas, and the gas pressure in the atomizing process is 2-6 MPa; the atomizing gas is preferably nitrogen or argon;
(4) And after the atomized flaky powder is completely cooled, taking down the powder collector for screening.
Example 1:
in the embodiment, the iron-based flaky powder material consists of 73% of Fe,25% of W and 2% of B by mass, and the preparation method of the iron-based flaky powder is carried out according to the following steps:
loading the intermediate alloy prepared from the mixed raw materials into an alumina crucible, carrying out resistance heating and stirring under the condition that the vacuum degree is less than 20Pa, melting under the condition that the superheat degree is 250-300 ℃, preserving heat for 1min, closing a vacuum system, pouring molten metal into a diversion crucible, pouring the molten metal into the diversion crucible with the diameter of a liquid guide pipe of 3mm, continuously flowing out along the liquid guide pipe on the diversion crucible, opening a nitrogen gas valve, keeping the gas pressure at 3.0+/-0.1 MPa, taking down a powder collector after atomized powder is completely cooled, and sieving to obtain the gas atomized flaky iron-based metal powder. The prepared powder is similar to a salix leaf shape, and has a diameter-thickness ratio of 50-200 and an oxygen content of less than 300ppm as shown in figure 1.
Example 2:
referring to the process steps of example 1, a sheet metal material was prepared, the mass percentages of the raw materials being Fe:30%, ni:60%, W:10%. The present embodiment differs from embodiment 1 in that: the crucible made of magnesium oxide is heated in an induction way, the vacuum degree is less than 100Pa, the superheat degree is 200-240 ℃, the temperature is kept for 10min, the atomizing medium is argon, and the gas pressure is 3.5+/-0.1 MPa. The prepared powder has a shape similar to that of a salix leaf, and has oxygen content less than 300ppm as shown in figure 2.
Example 3:
referring to the process steps of example 1, a sheet metal material was prepared, the mass percentages of the raw materials being Fe:30%, ni:55%, co:4%, al:1%, W:10%. The present embodiment differs from embodiment 1 in that: the vacuum degree is less than 50Pa, the resistance heating is carried out, the superheat degree is 150-190 ℃, the heat preservation is carried out for 20min, the atomizing medium is nitrogen, the gas pressure is 4.0+/-0.1 MPa, the diameter of a catheter is 8mm, and the oxygen content is less than 350ppm.
Example 4:
a sheet metal material was prepared with reference to the process steps of example 1, starting from pure Fe. The present embodiment differs from embodiment 1 in that: the vacuum degree is less than 100Pa, the induction heating is carried out, the superheat degree is 100-145 ℃, the heat preservation is carried out for 25min, the atomizing medium is nitrogen, the gas pressure is 5.0+/-0.1 MPa, the diameter of the catheter is 5mm, and the oxygen content is less than 400ppm.
Example 5:
a sheet metal material was prepared with reference to the process steps of example 1, starting from pure Cu. The present embodiment differs from embodiment 1 in that: vacuum degree is 30Pa, induction heating, superheat degree is 55-95 ℃, heat preservation is carried out for 30min, atomizing medium is argon, gas pressure is 5.6+/-0.1 MPa, diameter of a catheter is 6mm, and oxygen content is less than 250ppm.
The invention realizes low-cost and short-flow preparation of the flaky metal powder by adopting the gas atomization powder process, and is expected to realize industrialized batch production. By adopting the technical ideas of low superheat degree, high catheter aperture and low-pressure gas atomization, the viscosity of the atomized melt is improved, the energy input of the melt with unit mass is reduced, and the shape of the gas atomized powder is changed from spherical to lamellar. The obtained flaky metal powder has the advantages of large width-to-thickness dimension ratio, less impurities, large yield, low oxygen content and the like. The obtained sheet metal powder is in the shape of regular or irregular salix leaf with microcrystalline, nanocrystalline or amorphous structure.
The foregoing description of the preferred embodiments of the invention is merely illustrative of the invention and is not intended to be limiting. It should be noted that, for those skilled in the art, other equivalent modifications can be made in light of the technical teaching provided by the present invention, and the present invention can be implemented as the scope of protection.
Claims (3)
1. A method for preparing sheet metal powder, the method comprising:
(1) Heating, stirring and overheat preserving the metal raw material under the condition that the vacuum degree is less than 100Pa to obtain molten metal, wherein the overheat degree is 50-300 ℃, and the overheat preserving time is 1-30 min; the molten metal liquid consists of one or more elements in Fe, ni, W, al, cu, B, co;
(2) Pouring the molten metal liquid obtained in the step (1) into a diversion crucible, continuously flowing out along a liquid guide pipe on the diversion crucible, and introducing atomizing gas to atomize to obtain flaky powder; the guide crucible is made of aluminum oxide or magnesium oxide, the diameter of the liquid guide pipe is 3-8 mm, the atomizing gas is inert gas, and the gas pressure in the atomizing process is 2-6 MPa;
(3) And (3) completely cooling the flaky powder obtained in the step (2), and screening.
2. The method according to claim 1, wherein the step (1) heats the metal raw material by resistance heating or induction heating.
3. The method of claim 1, wherein the atomizing gas is nitrogen or argon.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4272463A (en) * | 1974-12-18 | 1981-06-09 | The International Nickel Co., Inc. | Process for producing metal powder |
| JPH03232909A (en) * | 1990-02-08 | 1991-10-16 | Daido Steel Co Ltd | Manufacture of metal powder |
| JP2001064704A (en) * | 1999-08-25 | 2001-03-13 | Kubota Corp | Method and device for manufacturing soft magnetic metal powder, soft magnetic metal powder, compacted body, and manufacture of compacted body |
| US6254661B1 (en) * | 1997-08-29 | 2001-07-03 | Pacific Metals Co., Ltd. | Method and apparatus for production of metal powder by atomizing |
| CN105290411A (en) * | 2014-05-28 | 2016-02-03 | 深圳市铂科新材料股份有限公司 | Method for lowering powder size and changing powder shape in atomization process of molten metal |
| CN110295294A (en) * | 2019-06-19 | 2019-10-01 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method mutually optimizing copper chromium contact by adding Ultra-fine Grained chromium |
| CN111804923A (en) * | 2020-07-15 | 2020-10-23 | 湖南省天心博力科技有限公司 | Preparation process of high-purity low-oxygen copper powder and water atomization device thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10593453B2 (en) * | 2016-07-25 | 2020-03-17 | Tdk Corporation | High permeability magnetic sheet |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4272463A (en) * | 1974-12-18 | 1981-06-09 | The International Nickel Co., Inc. | Process for producing metal powder |
| JPH03232909A (en) * | 1990-02-08 | 1991-10-16 | Daido Steel Co Ltd | Manufacture of metal powder |
| US6254661B1 (en) * | 1997-08-29 | 2001-07-03 | Pacific Metals Co., Ltd. | Method and apparatus for production of metal powder by atomizing |
| JP2001064704A (en) * | 1999-08-25 | 2001-03-13 | Kubota Corp | Method and device for manufacturing soft magnetic metal powder, soft magnetic metal powder, compacted body, and manufacture of compacted body |
| CN105290411A (en) * | 2014-05-28 | 2016-02-03 | 深圳市铂科新材料股份有限公司 | Method for lowering powder size and changing powder shape in atomization process of molten metal |
| CN110295294A (en) * | 2019-06-19 | 2019-10-01 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method mutually optimizing copper chromium contact by adding Ultra-fine Grained chromium |
| CN111804923A (en) * | 2020-07-15 | 2020-10-23 | 湖南省天心博力科技有限公司 | Preparation process of high-purity low-oxygen copper powder and water atomization device thereof |
Non-Patent Citations (2)
| Title |
|---|
| A. Ünal.Effect of processing variables on particle size in gas atomization of rapidly solidified aluminium powders.Materials Science and Technology .2013,第3卷第1029-1039页. * |
| 气体雾化技术制备金属粉末研究综述;朱盼星等;粉末冶金工业;第31卷(第4期);第82-87页 * |
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